Dimethylformamide → 4-(Chlorosulphonyl)benzoyl chloride

HRID 643997

반응식

HRID 643997 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 820244-(Chlorosulphonyl)benzoyl chloride

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-119c53acd0124ce789c798d70f4fa53c
출처 데이터셋
uspto-grants-2010_04
특허 번호
US07700637B2

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