Simple exploration of 4629-80-5

4629-80-5, The synthetic route of 4629-80-5 has been constantly updated, and we look forward to future research findings.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4629-80-5,1,3-Dimethylpiperidin-4-one,as a common compound, the synthetic route is as follows.

The 3-bromo-i-propoxybenzene (200 g, 0.08703 mol) was combined with THF (540 ml) under nitrogen and cooled to about -75 C. n-Butyl lithium (565 ml, 0.8306 mol) was added dropwise while maintaining the mixture at less than -70 C. After 2 hours 1,3-Dimethyl-4-piperidone (106.7 g, 0.8389 mol) was added while maintaining the temperature of the mixture between -80 C. and -70 C. After stirring 2 hours at -70 C., the reaction mixture was then added to 6N HCl (280 ml) while maintaining the temperature at 20-25 C. The pH was adjusted to 1 with 12 N HCl. The aqueous layer containing product was separated and heptane (320 ml) was added along with 50% NaOH (48 ml, pH=13-14) and the resulting mixture allowed to stand overnight. The mixture was heated to 45-50 C. and the upper layer was separated. The remaining aqueous layer was extracted with heptane (320 ml) at 45-50 C. The combined organic fractions were washed with de-ionized water (120 ml) at 45-50 C. The resulting organic layer was vacuum distilled at a pot temperature of about 55 C. at 100 mmHg. Crystallization from heptane and drying provided 151.8 g of 3-(3-i-propoxyphenyl)-1,3-dimethyl-4-hydroxypiperidine. Melting point 75.0- 76.0 C.

4629-80-5, The synthetic route of 4629-80-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Eli Lilly and Company; US5250542; (1993); A;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

 

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As the paragraph descriping shows that 4629-80-5 is playing an increasingly important role.

4629-80-5, 1,3-Dimethylpiperidin-4-one is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated,4629-80-5

The 3-bromo-i-propoxybenzene (200 g, 0.08703 mol) was combined with THF (540 ml) under nitrogen and cooled to about -75 C. n-Butyl lithium (565 ml, 0.8306 mol) was added dropwise while maintaining the mixture at less than -70 C. After 2 hours 1,3-Dimethyl-4-piperidone (106.7 g, 0.8389 mol) was added while maintaining the temperature of the mixture between -80 C. and -70 C. After stirring 2 hours at -70 C., the reaction mixture was then added to 6N HCl (280 ml) while maintaining the temperature at 20-25 C. The pH was adjusted to 1 with 12 N HCl. The aqueous layer containing product was separated and heptane (320 ml) was added along with 50% NaOH (48 ml, pH=13-14) and the resulting mixture allowed to stand overnight. The mixture was heated to 45 -50 C. and the upper layer was separated. The remaining aqueous layer was extracted with heptane (320 ml) at 45-50 C. The combined organic fractions were washed with de-ionized water (120 ml) at 45-50 C. The resulting organic layer was vacuum distilled at a pot temperature of about 55 C. at 100 mmHg. Crystallization from heptane and drying provided 151.8 g of 3-(3-i-propoxyphenyl)-1,3-dimethyl-4-hydroxypiperidine. Melting point 75.0-76.0 C.

As the paragraph descriping shows that 4629-80-5 is playing an increasingly important role.

Reference:
Patent; Eli Lilly and Company; US5159081; (1992); A;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

 

Simple exploration of 4629-80-5

4629-80-5, Big data shows that 4629-80-5 is playing an increasingly important role.

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4629-80-5,1,3-Dimethylpiperidin-4-one,as a common compound, the synthetic route is as follows.

B. Preparation of the Piperidinol The 3-bromo-i-propoxybenzene (200 g, 0.08703 mol) was combined with THF (tetrahydrofuran) (540 ml) under nitrogen and cooled to about -75 C. n-Butyllithium (565 ml, 0.8306 mol) was added dropwise while maintaining the mixture at less than -70 C. After 2 hours 1,3-dimethyl-4-piperidone (106.7 g, 0.8389 mol) was added while maintaining the temperature of the mixture between -80 C. and -70 C. After stirring for 2 hours at -70 C., the reaction mixture was then added to 6N HCl (280 ml) while maintaining the temperature at 20-25 C. The pH was adjusted to 1 with 12 N HCl. The aqueous layer was isolated and heptane (320 ml) was added to it along with 50% NaOH (48 ml, to pH of 13-14). The resulting mixture was allowed to stand overnight. The mixture was heated to 45-50 C. and the upper layer was separated. The remaining aqueous layer was extracted with heptane (320 ml) at 45-50 C. The combined organic fractions were washed with de-ionized water (120 ml) at 45-50 C. The resulting organic layer was vacuum distilled at a pot temperature of about 55 C. at 100 mmHg to remove part of the heptane. Crystallization from heptane provided 151.8 g of the named product. Melting point 75.0-76.0 C. Analysis: Calc. for (C16 H25 NO2): C, 72.97; H, 9.57; N, 5.32. Found: C, 72.87; H, 9.56; N, 5.25.

4629-80-5, Big data shows that 4629-80-5 is playing an increasingly important role.

Reference:
Patent; Eli Lilly and Company; US5136040; (1992); A;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

 

New learning discoveries about 4629-80-5

Big data shows that 4629-80-5 is playing an increasingly important role.

4629-80-5, 1,3-Dimethylpiperidin-4-one is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

EXAMPLE 14 6-chloro-3-(1,3-dimethyl-1,2,3,6-tetrahydropyridin-4-yl)-1H-indole Beginning with 0.97 gm (6.4 mMol) 6-chloro-1H-indole and 1.6 gm (13.0 mMol) 1,3-dimethyl-4-piperidone, 1.05 gm (63%) of the title compound were recovered as a crystalline solid. m.p.=170-172 C. MS(FD): m/e=260 (M+) EA: Calculated for: C15 H17 N2 Cl: Theory: C, 69.09; H, 6.57; N, 10.74. Found: C, 69.39; H, 6.40; N, 10.97., 4629-80-5

Big data shows that 4629-80-5 is playing an increasingly important role.

Reference:
Patent; Eli Lilly and Company; US5846982; (1998); A;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

 

Some tips on 4629-80-5

The synthetic route of 4629-80-5 has been constantly updated, and we look forward to future research findings.

4629-80-5, 1,3-Dimethylpiperidin-4-one is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

B. Preparation of the Piperidinol The 3-bromo-i-propoxybenzene (200 g, 0.08703 mol) was combined with THF (tetrahydrofuran) (540 ml) under nitrogen and cooled to about -75 C. n-Butyllithium (565 ml, 0.8306 mol) was added dropwise while maintaining the mixture at less than -70 C. After 2 hours 1,3-dimethyl-4-piperidone (106.7 g, 0.8389 mol) was added while maintaining the temperature of the mixture between -80 C. and -70 C. After stirring for 2 hours at -70 C., the reaction mixture was then added to 6N HCl (280 ml) while maintaining the temperature at 20-25 C. The pH was adjusted to 1 with 12 N HCl. The aqueous layer was isolated and heptane (320 ml) was added to it along with 50% NaOH (48 ml, to pH of 13-14). The resulting mixture was allowed to stand overnight. The mixture was heated to 45-50 C. and the upper layer was separated. The remaining aqueous layer was extracted with heptane (320 ml) at 45-50 C. The combined organic fractions were washed with de-ionized water (120 ml) at 45-50 C. The resulting organic layer was vacuum distilled at a pot temperature of about 55 C. at 100 mmHg to remove part of the heptane. Crystallization from heptane provided 151.8 g of the named product. Melting point 75.0-76.0 C. Analysis: Calc. for (C16 H25 NO2): C, 72.97; H, 9.57; N, 5.32. Found: C, 72.87; H, 9.56; N, 5.25., 4629-80-5

The synthetic route of 4629-80-5 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Eli Lilly and Company; US5136040; (1992); A;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

 

Brief introduction of 4629-80-5

As the paragraph descriping shows that 4629-80-5 is playing an increasingly important role.

4629-80-5,With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.4629-80-5,1,3-Dimethylpiperidin-4-one,as a common compound, the synthetic route is as follows.

EXAMPLE 14 6-chloro-3-(1,3-dimethyl-1,2,3,6-tetrahydropyridin-4-yl)-1H-indole Beginning with 0.97 gm (6.4 mMol) 6-chloro-1H-indole and 1.6 gm (13.0 mMol) 1,3-dimethyl-4-piperidone, 1.05 gm (63%) of the title compound were recovered as a crystalline solid. m.p.= 170-172C MS(FD): m/e=260 (M+) EA: Calculated for: C15H17N2Cl: Theory: C, 69.09; H, 6.57; N, 10.74. Found: C, 69.39; H, 6.40; N, 10.97.

As the paragraph descriping shows that 4629-80-5 is playing an increasingly important role.

Reference:
Patent; ELI LILLY AND COMPANY; EP812826; (1997); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem