Dimethylformamide → 4-(Chlorosulphonyl)benzoyl chloride

HRID 643997

反応式

HRID 643997 の反応式
[C:1](Cl)(=O)[C:2]([Cl:4])=[O:3].[Cl:7][S:8]([C:11]1[CH:19]=[CH:18]C(C(O)=O)=[CH:13][CH:12]=1)(=[O:10])=[O:9].CN(C=O)C>C(Cl)Cl>[Cl:7][S:8]([C:11]1[CH:19]=[CH:18][C:1]([C:2]([Cl:4])=[O:3])=[CH:13][CH:12]=1)(=[O:10])=[O:9]

参加物

5

反応物 3

HCID 6228DimethylformamideHCID 65578Oxalyl chlorideHCID 823854-(Chlorosulfonyl)benzoic acid

生成物 1

HCID 820244-(Chlorosulphonyl)benzoyl chloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

Oxalyl chloride (1.179 g, 9.29 mmol) is added to a suspension of 4-chlorosulfonyl-benzoic acid (1.025 g, 4.64 mmol) in 10 mL of DCM at RT. A drop of DMF is added. Stirring is continued for 2.5 days. A pale yellow solution results. The reaction mixture is concentrated under vacuum. Toluene is added and the mixture is concentrated under vacuum again. This last process is repeated twice more, and the mixture is finally dried under vacuum to give 4-chlorosulfonyl-benzoyl chloride as a pale yellow solid.

後処理

  1. customA pale yellow solution results
  2. concentrationThe reaction mixture is concentrated under vacuum
  3. additionToluene is added
  4. concentrationthe mixture is concentrated under vacuum again
  5. customthe mixture is finally dried under vacuum

出典と根拠

ORDレコード
ord-119c53acd0124ce789c798d70f4fa53c
出典データセット
uspto-grants-2010_04
特許番号
US07700637B2

関連ノート

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