Tag: M.W:300-400

61869-08-7, (3S,4R)-3-((Benzo[d][1,3]dioxol-5-yloxy)methyl)-4-(4-fluorophenyl)piperidine is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

61869-08-7, EXAMPLE 3 Preparation of paroxetine hydrochloride hemihydrate 11.58 kg of paroxetine free base was charged into a reactor containing 81.06 L of ethyl acetate and stirred for about 15 minutes at about 30 C. to form a clear solution. The reaction mass was filtered through a filtration system containing an online filter (5 micron polypropylene cloth), a 0.45 micron cartridge polypropylene filter, and a 0.2 micron cartridge polypropylene filter, and the filtration system was washed with 34.74 L of ethyl acetate. 2.895 L of 36% aqueous hydrochloric acid was added slowly to the filtrate over about 30 minutes at about 28-33 C. The reaction mass was stirred for about 1 hour, 45 minutes at about 28-30 C. It was then cooled to about 1 C. and maintained for about 1 hour, 30 minutes at about 0-2 C. The reaction mass was centrifuged and the wet cake washed with 23.16 L of chilled ethyl acetate. The wet solid was dried at 30 C. for about 1 hour, 15 minutes under a vacuum of about 690 mm Hg. The solid was further dried at about 58 C. under a vacuum of about 690 mm Hg for about 4 hours to get 10.9 kg of the paroxetine hydrochloride.; EXAMPLE 4 Purification of paroxetine hydrochloride hemihydrate 10.9 kg of the paroxetine hydrochloride obtained in Example 3 above was charged into a clean, dry reactor containing 76.3 L of acetone and the contents were heated to reflux. 4.564 L of water was added to the reaction suspension at reflux for about 60 minutes and stirred at reflux for about 20 minutes to form a clear solution. The reaction mass was cooled slowly to about 33 C. in 2 hours and then stirred for 1 hour at about 30-33 C. 32.7 L of n-heptane was charged into the reactor and stirring was continued for about 1 hour, 30 minutes. The reaction mass was cooled to about 2 C. and stirred for about 2 hours. The reaction mass was centrifuged and wet cake was washed with 6.54 L of chilled acetone. The wet solid was dried under vacuum of about 690 mm Hg at about 30 C. for about 2 hours and then at about 55-57 C. for about 4 hours. The resultant solid was milled in a micronizer (Manufacturer: Microtech Engineering company, Model: M-50) with an air pressure of 0.5 kg/cm2 at a feed rate of 7 kg/hour and then sieved through a 10 mesh sieve yielding 8.7 Kg of paroxetine hydrochloride hemihydrate with particle size distribution: D10=2.37 mum; D50=11.1 mum; and D90=30.6 mum.

61869-08-7 (3S,4R)-3-((Benzo[d][1,3]dioxol-5-yloxy)methyl)-4-(4-fluorophenyl)piperidine 44274603, apiperidines compound, is more and more widely used in various fields.

Reference：
Patent; Thippannachar, Vijayavitthal Mathad; Jayantilal, Pravinchandra Vankawala; Elati, Chandrasekhar Ravi Ram; Kolla, Naveen Kumar; Chlamala, Subrahmanyeswara Rao; US2006/264637; (2006); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.61869-08-7,(3S,4R)-3-((Benzo[d][1,3]dioxol-5-yloxy)methyl)-4-(4-fluorophenyl)piperidine,as a common compound, the synthetic route is as follows.,61869-08-7

203-L isopropanol (water 0. 05% w/v) and 13.5 Kg Paroxetine base are charged simultaneously in a reactor and stirred for 15 min to get clear solution. The solution is filtered through sparkler filter to remove suspended particles. The reactor and sparkler filters are washed with 2 x 13.5-L isopropanol. The filtrate and washing solutions are collected into a glass-lined reactor. To this solution of Paroxetine base a solution of 20% w/v hydrogen chloride in isopropanol is added from addition funnel during 120 minutes at 30-35C to bring the pH of the reaction mass between 3-4 (checked on pH paper), at this pH Paroxetine hydrochloride crystallizes. The slurry is stirred for 15 minutes and then slowly heated to 80-82C, 135 L isopropanol is distilled off at atmospheric pressure and then cooled. The product crystallized out at 45C, which is then further cooled to 30-35C and stirred for 1 hr at this temperature. The product is centrifuged and washed with 2 x 13.5-L isopropanol. The wet cake is then transferred to a vacuum tray dryer. The product is dried at 30-35C for 2 hrs, at 50-55C for 6 hrs and finally at 70-75C for 12 hrs under reduced pressure of 30 mm, reducing isopropanol content to less than 3%. The yield of anhydrous Paroxetine hydrochloride is 13.5 Kg Water content of distillate 0.6% Melting point 116-117C Purity (by HPLC) 99.72% Water (by KFR) 1.48% isopropanol (by GC) 2.4%; Example 2 20 g of Paroxetine base is dissolved in 360-ml isopropanol (water <0.05%). The solution is filtered through filter pad in Buchner funnel. The pad is washed twice with 20-ml isopropanol. To the clear filtrate is added 20% w/v hydrogen chloride solution in isopropanol at 30-35C to bring the pH of the reaction mass between 3-4 (checked on pH paper). Paroxetine hydrochloride is CRYSTALLISED out. The slurry is stirred for 15 minutes and then slowly heated to 80-82C to obtain a clear solution, which is then subjected to distillation for the removal of 200 ml isopropanol at atmospheric pressure. The solution is then cooled and the product crystallised out at 30-35C. Slurry thus obtained is stirred for 1 hr at the same temperature. The product is filtered and washed with 4 x 20-ml isopropanol. The wet cake is dried in vacuum oven at 65C for 4 hrs and between the range 70-75C for 16 hrs under reduced pressure of 30 mm to afford 19.9 g Paroxetine hydrochloride. Melting point 116-117C Water content of distillate 0.55% Purity by HPLC 99.96%, Isopropanol (by GC) 2.96% Water (by KFR) 1.5%; Example 3 20 g of Paroxetine base is dissolved in 360-ml isopropanol (water <0.05%). The solution is filtered through filter pad in Buchner funnel. The pad is washed twice with 20 ml isopropanol. To the clear filtrate is added 20% hydrogen chloride solution in isopropanol at 30-35C to bring the pH of the reaction mass between 3-4 (checked on pH paper). Paroxetine hydrochloride is crystallized out at this pH. The slurry is stirred for 15 min. and then slowly heated to 80-82C to obtain a clear solution, which is then subjected to distillation for removal of 200 ml isopropanol at atmospheric pressure. The solution is then cooled to 30 to 35 C and the product crystallized out. The slurry thus obtained is stirred for 1 hour. The product is filtered and washed with 4 x 20-ml isopropanol. The wet cake is dried in vacuum oven between the range 70-75C for 16 hrs under reduced pressure of 30 mm to afford 19.5 g of Paroxetine hydrochloride. Melting point 116-117C Water content of distillate 0.6% Purity by HPLC 99.96%, Isopropanol (by GC) 2.18% Water (by KFR) 1.46% The synthetic route of 61869-08-7 has been constantly updated, and we look forward to future research findings. Reference：
Patent; CADILA HEALTHCARE LIMITED; WO2005/19209; (2005); A2;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.220394-97-8,1-Boc-4-(Cbz-amino)piperidine,as a common compound, the synthetic route is as follows.

A solution of 4-benzyloxycarbonylamino-piperidine-l-carboxylic acid tert-butyl ester (17.73 g, 53 mmol) in trifluoroacetic acid (30 ml) was stirred at room temperature for 30 min. The solvent was removed under reduced pressure and the residue was partitioned between IN aq, sodium hydroxide (30 ml) and a DCM-MeOH mixture (9-1, 100 ml). The aq. layer was extracted four more times with the same mixture. The combined extracts were dried over sodium sulfate, filtered and concentrated to dryness. The residue was chromatographed (DCM-MeOH 9-1 1% aq. ammonium hydroxide then DCM-MeOH 4-1) to afford the title piperidine (11.03 g, 47.07 mmol). .H NMR (CDC13) 8: 7.40-7.29 (m, 5H); 6.19 (br. s, 1H); 5.10 (s, 2H); 5.04 (s, 1H); 3.47 (m, 1H); 3.25 (br. d, J= 12.8 Hz, 2H); 2.81 (t, J= 12 Hz, 2H); 2.04 (m, 2H); 1.58 (m,2H)., 220394-97-8

220394-97-8 1-Boc-4-(Cbz-amino)piperidine 1514305, apiperidines compound, is more and more widely used in various fields.

Reference：
Patent; ACTELION PERCUREX AG; WO2006/99884; (2006); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.61869-08-7,(3S,4R)-3-((Benzo[d][1,3]dioxol-5-yloxy)methyl)-4-(4-fluorophenyl)piperidine,as a common compound, the synthetic route is as follows.,61869-08-7

0.8 g of oily paroxetine free base and 1.31 g of taurocholic acid were completely dissolved in a mixed solvent of purified water (5 mL) and ethanol (20 mL) while heating to 40 C. with shaking for one hour. After the solution was concentrated under reduced pressure until about 5 mL of the solvent was left, it was allowed to stand at -20 C.0 C. for 24 hours to precipitate a crystal, followed by filtration. The filtered residue was washed with cold methanol at 0 C. or less, and dried under vacuum to give 1.8 g of solid paroxetine taurocholate as a light gray powder.

The synthetic route of 61869-08-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Lee, Sang Joon; Shin, Hee Jong; Ki, Min Hyo; Lee, Su Kyoung; Kim, Bok Young; Lee, Hong Woo; US2006/63747; (2006); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1211587-42-6,Benzyl 4-((chlorosulfonyl)methyl)piperidine-1-carboxylate,as a common compound, the synthetic route is as follows.

Into a 100-mL round-bottom flask, was placed dichloromethane (30 mL), 2,2,2- trichloroethyl N-[(1R,3S,5S)-8-azabicyclo[3.2.1]octan-3-yl]carbamate (2.4 g, 7.96 mmol, 1.00 equiv), TEA (3.2 g, 31.62 mmol, 3.97 equiv). Then benzyl 4- [(chlorosulfonyl)methyl]piperidine-1-carboxylate (4 g, 12.05 mmol, 1.51 equiv) was added by dropwise at 0oC. The resulting solution was stirred for 12 h at 10oC. The resulting mixture was washed with 3×30 mL of water and 1×30 mL of brine. The mixture was dried over anhydrous sodium sulfate and concentrated under vacuum. The residue was applied onto a silica gel column with dichloromethane/methanol (20:1). This resulted in 2.8 g (59%) of benzyl 4-[[(1R,3S,5S)-3-[[(2,2,2-trichloroethoxy)carbonyl]amino]-8- azabicyclo[3.2.1]octane-8-sulfonyl]methyl]piperidine-1-carboxylate as a yellow solid

1211587-42-6, As the paragraph descriping shows that 1211587-42-6 is playing an increasingly important role.

Reference：
Patent; Epizyme, Inc.; Poley, Megan Allen Clunan; Kunz, Kevin Wayne; Mills, James Edward John; Mitchell, Lona Helen; munckhof, Michael John; Harvey, Darren Martin; (303 pag.)KR2017/45749; (2017); A;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

479636-65-2, 8-tert-Butyl 3-ethyl 1-oxa-2,8-diazaspiro[4.5]dec-2-ene-3,8-dicarboxylate is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Compound 7-b (0.10 g, 0.32 mmol) was dissolved in methylene chloride (2 mL), 4N hydrogen chloride dioxane solution (2 mL) was added, and the mixture was stirred at room temperature for 1 hour. After completion of the reaction, the solvent was removed to obtain the title compound 7-c (80 mg) as a beige solid, which was used for the next reaction without further purification., 479636-65-2

As the paragraph descriping shows that 479636-65-2 is playing an increasingly important role.

Reference：
Patent; Rego Kem Bio Between Eonseu Co., Ltd.; Lee Dae-yeon; Chae Sang-eun; Jeong Eun-mi; Yang Eun-hye; Choi Yun-jeong; Jeong Cheol-ung; Shin Ju-hyeon; Kim Yun-gi; Kwon Hyeon-jin; Ryu Jeong-hui; Ban Eun-hye; Kim Yong-ju; Oh Yeong-su; Chae Je-uk; (140 pag.)KR101798840; (2017); B1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

220394-97-8, 1-Boc-4-(Cbz-amino)piperidine is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

To a solution of compound I-4 (470 mg, 1.47 mmol) in DCM, TFA (2.5 mL, 29 mmol) was addedand then the reaction mixture was stirred at room temperature for 2 h and then was evaporated togive the crude product directly used in the next step A mixture of the amine, DIEA (3.84 mL,22.05mmol) and cyclohexanone (1.5 mL) in THF (10 mL) was stirred at room temperature for 1.5h and then NaBH(OAc)3 (1.6 g, 7.35 mmol) was added into the solution. The reaction mixture wasstirred at room temperature for overnight and then H2O was added to quench the reaction. Thesolution was extracted with ethyl acetate (30 mL × 2). The organic layer was washed with brine(15 mL × 2) and then was dried over anhydrous MgSO4. After filtration and concentration, thecrude product I-5 was obtained and purified with column chromatography ( methylene chloride/methanol = 45:1 to 30:1) to give compound I-5 as light yellow oil (350 mg, 78%)., 220394-97-8

As the paragraph descriping shows that 220394-97-8 is playing an increasingly important role.

Reference：
Article; Zhou, Jie; Ji, Ming; Zhu, Zhixiang; Cao, Ran; Chen, Xiaoguang; Xu, Bailing; European Journal of Medicinal Chemistry; vol. 132; (2017); p. 26 – 41;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

61869-08-7, (3S,4R)-3-((Benzo[d][1,3]dioxol-5-yloxy)methyl)-4-(4-fluorophenyl)piperidine is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

1.0 g of oily paroxetine free base and 1.24 g of cholic acid were completely dissolved in a mixed solvent of ethanol (30 mL) and dichloromethane (50 mL) while heating to 50 C. with shaking for 3 hours. After the solution was distilled under reduced pressure to remove the dichloromethane, it was allowed to stand at 25 C. for 8 hours, filtered, and dried under vacuum to yield 1.94 g of solid paroxetine cholate as a white crystal.

61869-08-7, The synthetic route of 61869-08-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Lee, Sang Joon; Shin, Hee Jong; Ki, Min Hyo; Lee, Su Kyoung; Kim, Bok Young; Lee, Hong Woo; US2006/63747; (2006); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

873779-30-7, tert-Butyl 5-bromo-2-oxospiro[indoline-3,4′-piperidine]-1′-carboxylate is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,873779-30-7

To R8, purchased from ACTIVATE (150 mg, 0.39 mmol) in dichloromethane (3 mL) is added trifluoroacetic acid (0.5 mL) and reaction mixture is stirred for 45 minutes at r.t. The reaction mixture is concentrated. Yield 100%.

As the paragraph descriping shows that 873779-30-7 is playing an increasingly important role.

Reference：
Patent; Boehringer Ingelheim International GmbH; VINTONYAK, Viktor; GRAUERT, Matthias; GRUNDL, Marc; PAUTSCH, Alexander; (64 pag.)US2016/75704; (2016); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

61869-08-7, (3S,4R)-3-((Benzo[d][1,3]dioxol-5-yloxy)methyl)-4-(4-fluorophenyl)piperidine is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

1.0 g of oily paroxetine free base and 1.24 g of cholic acid were completely dissolved in 10 mL of N,N-dimethylacetamide while heating to 40 C. with shaking for 20 minutes. The solution was slowly added dropwise to 100 mL of ethyl ether to precipitate a solid, stirred at 0 C. for 3 hours, and filtered. The filtered residue was washed with 30 mL of ethyl ether, and dried under vacuum to yield 1.75 g of solid paroxetine cholate as a light gray powder., 61869-08-7

The synthetic route of 61869-08-7 has been constantly updated, and we look forward to future research findings.

Reference：
Patent; Lee, Sang Joon; Shin, Hee Jong; Ki, Min Hyo; Lee, Su Kyoung; Kim, Bok Young; Lee, Hong Woo; US2006/63747; (2006); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem