Oxalyl chloride → 1-Methylpiperidine-4-carbonyl chloride hydrochloride

HRID 245714

반응식

HRID 245714 반응식
[ClH:1].[CH3:2][N:3]1[CH2:8][CH2:7][CH:6]([C:9](O)=[O:10])[CH2:5][CH2:4]1.C(Cl)(=O)C([Cl:15])=O>ClCCl.CN(C)C=O>[ClH:15].[CH3:2][N:3]1[CH2:8][CH2:7][CH:6]([C:9]([Cl:1])=[O:10])[CH2:5][CH2:4]1

참가 물질

5

반응물 2

HCID 65578Oxalyl chlorideHCID 27600434-Piperidinecarboxylic acid, 1-methyl-, hydrochloride (1:1)

생성물 1

HCID 219565061-Methylpiperidine-4-carbonyl chloride hydrochloride수율 111.1%

시약·촉매·용매 2

HCID 6228Dimethylformamide촉매HCID 6344Dichloromethane용매

실험 절차

To a suspension of 1-methyl-piperidine-4-carboxylic acid hydrochloride (11.36 mmol, 2.04 g) and N,N-dimethylformamide (0.129 mmol, 0.01 ml, 9.40 mg) in dichloromethane (10 ml) at 0° C. was added oxalyl chloride (14.76 mmol, 1.40 ml) drop wise. The cooling bath was removed and the reaction mixture stirred at room temperature for 20 hours. Then the reaction mixture was concentrated in vacuo to give 1-methylpiperidine-4-carbonyl chloride hydrochloride (2.5 g).

후처리

  1. customThe cooling bath was removed
  2. concentrationThen the reaction mixture was concentrated in vacuo

출처 및 근거

ORD 기록
ord-5c63cbcfa90a49bcbd1a3c66ee2477c2
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08658794B2

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