Thionyl Chloride → 4-(N,N-diethylcarbamoyl)benzhydryl chloride

HRID 929652

反応式

HRID 929652 の反応式
[CH2:1]([N:3]([CH2:20][CH3:21])[C:4]([C:6]1[CH:19]=[CH:18][C:9]([CH:10](O)[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:8][CH:7]=1)=[O:5])[CH3:2].S(Cl)([Cl:24])=O>ClCCl>[CH2:1]([N:3]([CH2:20][CH3:21])[C:4]([C:6]1[CH:19]=[CH:18][C:9]([CH:10]([Cl:24])[C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:8][CH:7]=1)=[O:5])[CH3:2]

参加物

4

反応物 2

HCID 24386Thionyl ChlorideHCID 105409664-(N,N-diethylcarbamoyl)benzhydryl alcohol

生成物 1

HCID 107330954-(N,N-diethylcarbamoyl)benzhydryl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

The 4-(N,N-diethylcarbamoyl)benzhydryl alcohol (61.35 g, 216.5 mmol) was dissolved in 1500 mL of dichloromethane and 23.69 mL (324.8 mmol) of thionyl chloride was added dropwise. The reaction solution was stirred overnight at room temperature and the solvent was removed under vacuum. The crude product was redissolved in 800 mL of toluene and the solvent again was removed under vacuum to eliminate excess thionyl chloride, providing crude 4-(N,N-diethylcarbamoyl)benzhydryl chloride as a dark oil. Crude yield=100%.

後処理

  1. customthe solvent was removed under vacuum
  2. dissolutionThe crude product was redissolved in 800 mL of toluene
  3. customthe solvent again was removed under vacuum

出典と根拠

ORDレコード
ord-401efd2cf8fd4a3e9b6248fbbcc7eb6f
出典データセット
uspto-grants-2016_03
特許番号
US09296707B2

関連ノート

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