4-Chlorobenzamide → 4-Chlorothiobenzamide

HRID 477893노트

반응식

HRID 477893 반응식
[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

참가 물질

4

반응물 2

HCID 120844-ChlorobenzamideHCID 87949Lawesson's reagent

생성물 1

HCID 27348264-Chlorothiobenzamide수율 64%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-c402f6db24194e82a44b28f7d79f25dd
출처 데이터셋
uspto-grants-1989_12
특허 번호
US04889867

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