Hydrochloric Acid → 4-Chlorothiobenzamide

HRID 463882ノート

反応式

HRID 463882 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][CH:3]=1.C(N)(=[S:12])C.Cl>CN(C)C=O>[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]([NH2:7])=[S:12])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 121634-ChlorobenzonitrileHCID 2723949Thioacetamide

生成物 1

HCID 27348264-Chlorothiobenzamide収率 70.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 55.03 g of 4-chlorobenzonitrile, 75.13 g of thioacetamide and 600 ml of dimethylformamide was saturated with dry hydrogen chloride gas while being chilled in an ice bath. The mixture was then distilled slowly on an oil bath at 100° C. When the liquid had been removed, aqueous sodium bicarbonate was added. The solid was collected and recrystallized from toluene, giving 48.35 g of 4-chlorothiobenzamide as yellow crystals.

後処理

  1. temperaturewhile being chilled in an ice bath
  2. distillationThe mixture was then distilled slowly on an oil bath at 100° C
  3. customWhen the liquid had been removed
  4. additionaqueous sodium bicarbonate was added
  5. customThe solid was collected
  6. customrecrystallized from toluene

出典と根拠

ORDレコード
ord-779b64027b4342e8b5465d74100591ca
出典データセット
uspto-grants-1985_10
特許番号
US04544759

反応ノート

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