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

HRID 245714

反応式

HRID 245714 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 219565061-Methylpiperidine-4-carbonyl chloride hydrochloride収率 111.1%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide触媒HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-5c63cbcfa90a49bcbd1a3c66ee2477c2
出典データセット
uspto-grants-2014_02
特許番号
US08658794B2

関連ノート

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