N-BOC-3-Aminopiperidine synthesis
- Product Name:N-BOC-3-Aminopiperidine
- CAS Number:184637-48-7
- Molecular formula:C10H20N2O2
- Molecular Weight:200.28
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184637-48-7
In a 200 mL four-necked flask equipped with a stirrer, pH sensor, and two dropping funnels, 90 g of ethanol and 10.0 g (0.1 mol) of 3-aminopiperidine were added and stirred at 10 to 15 °C. 21.8 g (0.1 mol) di-tert-butyl dicarbonate was slowly added through one dropping funnel while 17.6 g (0.11 mol) 25% aqueous sodium hydroxide was added dropwise through the other dropping funnel, and the dropping rate was controlled to maintain the pH of the reaction system between 11.8 and 12.2. The titration process was completed in about 1 hour. Upon completion of the reaction, the composition of the reaction mixture was analyzed and confirmed to contain 6% unreacted 3-aminopiperidine, 91.5% of the target product 3-amino-1-tert-butoxycarbonylpiperidine and 1.1% of the by-product 3-tert-butoxycarbonylaminopiperidine.
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Yield:184637-48-7 97%
Reaction Conditions:
with palladium 10% on activated carbon;hydrogen in methanol at 45; for 3 h;Cooling with ice;
Steps:
5 5. Preparation of (R) -piperidine-3-ylcarbamic acid tert-butyl ester:
In an ice bath, 247 g of (R)-(1-benzylpiperidin-3-yl) carbamic acid tert-butyl ester (851 mmmol), 2470 g of methanol and 5 g of palladium carbon (10 w%) were added to a three-necked reaction flask;Hydrogen was replaced 3 times, and then the system was raised to 45 ° C for 3h; the reaction was monitored by TLC.The system was cooled to room temperature, filtered, and the filtrate was concentrated to dryness to obtain 165 g of tert-butyl (R) -piperidin-3-ylcarbamate (purity 95%; yield 97%).
References:
Suzhou Hande Chuanghong Biochemical Technology Co., Ltd.;Mao Zhongping;Ma Dongxu;Wei Hua CN110372573, 2019, A Location in patent:Paragraph 0068-0071
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