Benzenesulfonyl chloride, 4-chloro-3-nitro- → 3-amino-4-chlorobenzenethiol

HRID 1512972노트

반응식

HRID 1512972 반응식
[Sn].[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([S:9](Cl)(=O)=O)=[CH:5][C:4]=1[N+:13]([O-])=O>Cl>[Cl:2][C:3]1[CH:8]=[CH:7][C:6]([SH:9])=[CH:5][C:4]=1[NH2:13]

참가 물질

4

반응물 2

HCID 7323Benzenesulfonyl chloride, 4-chloro-3-nitro-HCID 5352426Tin atom

생성물 1

HCID 6406993-amino-4-chlorobenzenethiol수율 73.9%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

To a mixture of concentrated hydrochloric acid (30 mL) and ice (25 g) was added tin (29.7 g) under ice-cooling, followed by adding 4-chloro-3-nitrobenzenesulfonyl chloride (6.4 g), and the mixture was stirred under ice-cooling for 1.5 hours, and then stirred at 90° C. for 2 hours. The insoluble material was removed by filtration, and the filtrate was stirred at room temperature overnight. The precipitated crystals were collected by filtration. The collected crystals were washed with water, and dried under reduced pressure to give the title compound (2.95 g).

후처리

  1. temperaturecooling
  2. temperaturecooling for 1.5 hours
  3. stirringstirred at 90° C. for 2 hours
  4. customThe insoluble material was removed by filtration
  5. stirringthe filtrate was stirred at room temperature overnight
  6. filtrationThe precipitated crystals were collected by filtration
  7. washThe collected crystals were washed with water
  8. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-53fa4a2a38bf49118caa5aeffe7e6413
출처 데이터셋
uspto-grants-2012_07
특허 번호
US08217069B2

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