4-Chlorobenzamide → 4-Chlorothiobenzamide

HRID 477893ノート

反応式

HRID 477893 の反応式
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=O)=[CH:4][CH:3]=1.COC1C=CC(P2(=S)SP(=S)(C3C=CC(OC)=CC=3)[S:20]2)=CC=1>C1(C)C=CC=CC=1>[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([NH2:8])=[S:20])=[CH:4][CH:3]=1

参加物

4

反応物 2

HCID 120844-ChlorobenzamideHCID 87949Lawesson's reagent

生成物 1

HCID 27348264-Chlorothiobenzamide収率 64%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a stirred mixture of 14.9 grams (0.102 mole) of 4-chlorobenzamide in 800 ml of toluene was added 20.6 grams (0.051 mole) of 2,4-bis(4-methoxyphenyl)-1,3-dithia-2,4-diphosphetane-2,4-disulfide (Lawesson's Reagent). This mixture was stirred and heated at reflux for two hours. The reaction mixture was allowed to cool slowly to room temperature. Approximately 600 ml of toluene was evaporated from the mixture under reduced pressure, leaving a residual liquid. This liquid was purified by column chromatography on silica gel, eluting with methylene chloride:ethyl acetate (60:40), to yield 5.6 grams of 4-chlorophenylthiocarboxamide as a solid.

後処理

  1. temperatureheated
  2. temperatureat reflux for two hours
  3. customApproximately 600 ml of toluene was evaporated from the mixture under reduced pressure
  4. customleaving a residual liquid
  5. customThis liquid was purified by column chromatography on silica gel
  6. washeluting with methylene chloride:ethyl acetate (60:40)

出典と根拠

ORDレコード
ord-c402f6db24194e82a44b28f7d79f25dd
出典データセット
uspto-grants-1989_12
特許番号
US04889867

反応ノート

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