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

HRID 1512972ノート

反応式

HRID 1512972 の反応式
[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]

参加物

4

反応物 2

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

生成物 1

HCID 6406993-amino-4-chlorobenzenethiol収率 73.9%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-53fa4a2a38bf49118caa5aeffe7e6413
出典データセット
uspto-grants-2012_07
特許番号
US08217069B2

反応ノート

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