Hydrochloric Acid → 4-Methoxybenzenecarbothioamide

HRID 463884

反応式

HRID 463884 の反応式
[C:1](#[N:10])[C:2]1[CH:7]=[CH:6][C:5]([O:8][CH3:9])=[CH:4][CH:3]=1.C(N)(=[S:13])C.Cl>CN(C)C=O>[CH3:9][O:8][C:5]1[CH:6]=[CH:7][C:2]([C:1]([NH2:10])=[S:13])=[CH:3][CH:4]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 701294-MethoxybenzonitrileHCID 2723949Thioacetamide

生成物 1

HCID 7368274-Methoxybenzenecarbothioamide収率 75.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 53.26 g of anisonitrile and 60.10 g of thioacetamide in 600 ml of dimethylformamide was saturated with dry hydrogen chloride gas while being cooled in an ice bath. The mixture was then distilled on an oil bath at 100° C. After the liquid had been removed, aqueous sodium bicarbonate was added and the solid was collected and recrystallized from toluene, giving 50.47 g of 4-methoxythiobenzamide as a yellow solid.

後処理

  1. temperaturewhile being cooled in an ice bath
  2. distillationThe mixture was then distilled on an oil bath at 100° C
  3. customAfter 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-e79458266d034204a700be91ab1937be
出典データセット
uspto-grants-1985_10
特許番号
US04544759

関連ノート

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