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PIPERIDIN-3-YLMETHYL-CARBAMIC ACID BENZYL ESTER-HCl synthesis

3synthesis methods
1-Boc-3-(Cbz-aMinoMethyl)piperidine

478366-01-7
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PIPERIDIN-3-YLMETHYL-CARBAMIC ACID BENZYL ESTER-HCl

676621-99-1
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Yield:676621-99-1 84%

Reaction Conditions:

with hydrogenchloride in 1,4-dioxane at 0; for 1.33333 h;

Steps:

4.B

Part B: Preparation of 3-(Benzyloxycarbonylaminomethyl)-piperidine Hydrochloride A solution of 3-(benzyloxycarbonylaminomethyl)-piperidine-1-carboxylic acid tert-butyl ester (594 mg, 1.7 mmol) in ethyl acetate (10 mL) was stirred on an ice bath and treated with a solution of hydrogen chloride in dioxane (4.0 N, 10 mL, 40 mmol). The mixture was stirred for 80 minutes, then was concentrated under vacuum. The gummy residue was triturated repeatedly in ether to provide a white powder (408 mg, 84%)which was extremely hygroscopic and was used without further purification. 1H NMR (300 MHz, CD3OD) δ 7.34 (m, 5H), 5.07 (s, 2H), 3.34 (m, 2H), 3.09 (m, 2H), 2.88 (m, 1H), 2.66 (m, 1H), 1.90 (m, 3H), 1.70 (m, 1H), 1.30 (m, 1H).

References:

US2004/67935,2004,A1 Location in patent:Page/Page column 31