Dimethylformamide → 1-Methylpiperidine-4-carbonyl chloride

HRID 30804

反応式

HRID 30804 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([C:8]([OH:10])=O)[CH2:4][CH2:3]1.CN(C)C=O.C(Cl)(=O)C([Cl:19])=O>C(Cl)Cl>[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([C:8]([Cl:19])=[O:10])[CH2:4][CH2:3]1

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 27369391-Methylpiperidine-4-carboxylic acid

生成物 1

HCID 4365031-Methylpiperidine-4-carbonyl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

反応条件

温度
20 °C

実験手順

A flask was flame dried and placed under a nitrogen atmosphere. 1-methylpiperidine-4-carboxylic acid (1 eq) in anhydrous methylene chloride added to flask and cooled to 20° C. in a water bath. Dimethylformamide added, then oxalyl chloride (1.4 eq) in methylene chloride. Reaction refluxed for 2 hours, brought to room temperature, concentrated and azeotroped with toluene to yield 1-methylpiperidine-4-carbonyl chloride as a light yellow fluffy solid. MS: MH+=162.

後処理

  1. temperatureA flask was flame
  2. customdried
  3. customReaction
  4. temperaturerefluxed for 2 hours
  5. custombrought to room temperature
  6. concentrationconcentrated
  7. customazeotroped with toluene

出典と根拠

ORDレコード
ord-fa13b4bfb2d4459d835da3c9b478d77a
出典データセット
uspto-grants-2008_09
特許番号
US07423150B2

関連ノート

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