Phenyl chloroformate → HCID 13825039、化合物

HRID 648502ノート

反応式

HRID 648502 の反応式
[C:1](Cl)(=[O:9])[O:2][C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1.[Cl:11][CH:12]1[CH2:17][CH2:16][N:15](C)[CH2:14][CH2:13]1>C(Cl)Cl>[Cl:11][CH:12]1[CH2:17][CH2:16][N:15]([C:1]([O:2][C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)=[O:9])[CH2:14][CH2:13]1

参加物

4

反応物 2

HCID 15891Phenyl chloroformateHCID 793424-chloro-N-methylpiperidine

生成物 1

HCID 13825039HCID 13825039、化合物収率 71.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

A solution of phenyl chlorocarbonate (17.3 g) in dry methylene chloride (40 ml) was dropwise added to a stirred solution of 4-chloro-1-methylpiperidine (13.3 g) in dry methylene chloride (60 ml) under ice-cooling over a period of 5 minutes. The resultant mixture was stirred at the same temperature for 30 minutes and then at room temperature for 6 hours. The mixture was washed with water, dried over magnesium sulfate, and concentrated in vacuo to give an oil, which was distilled to give phenyl 4-chloro-1-piperidine-carboxylate (17.0 g) as a colourless oil.

後処理

  1. temperaturecooling over a period of 5 minutes
  2. washThe mixture was washed with water
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customto give an oil, which
  6. distillationwas distilled

出典と根拠

ORDレコード
ord-6a1cf50a9ac142f78cea1743e926d14b
出典データセット
uspto-grants-1988_04
特許番号
US04735952

反応ノート

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