Category: 1445-73-4

With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.1445-73-4,1-Methyl-4-piperidone,as a common compound, the synthetic route is as follows.

Pd/C (40 g, 5% w/w) was added into a 10 L autoclave reactor at room temperature under nitrogen. THF (2 L), 2 L of methylamine (27%-30% alcoholic solution, 2.1 eq.), and 800 g of compound 10A (7 mol, 1.0 eq.) were sequentially added into the reactor. The system was purged with hydrogen three times. The mixture was stirred at hydrogen pressure (50 psi) at 70-75 C overnight and was then filtered using a Biichner funnel and filter paper (pore size: 30-50 pm) over 10 minutes to remove the Pd/C. The filtrate was concentrated in a rotavapor under vacuum (30-40 mmHg) at 45-50 C for about 3 hours to obtain 933 g of yellow oil. The mixture was distilled without a column at atmospheric pressure and the 140-170 C portion was collected to obtain 763 g of compound 10 as a colorless oil (98.6% purity (AUC by HPLC, retention time = 4.8 minutes); 84.2% yield; 8000 ppm residual ethanol). A portion of the oil (563 g) was distilled using a 3 cm column at atmospheric pressure and the 140-170 C portion was collected to obtain 510 g of compound 10 (75.8% yield; 134 ppm residual ethanol). 1H- NMR (400 MHz, CDCb): d = 0.82 (bs, 1H), 1.10-1.12 (q, 2H), 1.66 (d, 2H), 1.73-1.81 (t, 2H), 2.05 (s, 3H), 2.08-2.19 (m, 1H), 2.22 (s, 3H), 2.60 (d, 2H). [00134] Step 10: Synthesis of HM04 fumarate salt, 1445-73-4

Big data shows that 1445-73-4 is playing an increasingly important role.

Reference：
Patent; HELSINN THERAPEUTICS (US) INC; HELSINN HEALTHCARE SA; HELSINN ADVANCED SYNTHESIS SA; RUBIO, Silvina Garcia; PERSEGHINI, Mauro; GUAINAZZI, Angelo; PIETRA, Claudio; GIULIANO, Claudio; (110 pag.)WO2019/118298; (2019); A1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem

1445-73-4, 1-Methyl-4-piperidone is a piperidines compound, ?involved in a variety of chemical synthesis. Rlated chemical reaction is continuously updated

Step 1 Preparation of 1-methyl-4-methylaminopiperidine A mixture of 1-methyl-4-piperidone (20 g, 0.18 mol) in methanol:tetrahydrofuran (100 mL, 1:1) and methyl amine (2 M in tetrahydrofuran, 3 mole excess) was placed in a Parr shaker with 5% Pd/C and hydrogenated for two hours at 60 psi and 70 C. The catalyst was filtered and the filtrate concentrated on the rotary evaporator. The crude material was distilled at 44-45 C. at 0.3 mm Hg to give 20 g (87%) of 1-methyl-4-methylaminopiperidine. Anal. Calc’d for C7H16N2: C, 65.57; H, 12.58; N, 21.85. Found: C, 65.49; H, 12.44; N: 21,49.

1445-73-4, As the paragraph descriping shows that 1445-73-4 is playing an increasingly important role.

Reference：
Patent; G. D. Searle & Company; US6423713; (2002); B1;; ; Patent; G.D. Searle & Company; US6514977; (2003); B1;,
Piperidine – Wikipedia
Piperidine | C5H11N – PubChem