Thionyl Chloride → N-benzylidene-4-trifluoromethylbenzenecarbohydrazonoyl chloride

HRID 1354413

반응식

HRID 1354413 반응식
[CH:1](=[N:8][NH:9][C:10](=O)[C:11]1[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][CH:12]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.S(Cl)([Cl:24])=O>C1(C)C=CC=CC=1>[CH:1](=[N:8][N:9]=[C:10]([Cl:24])[C:11]1[CH:16]=[CH:15][C:14]([C:17]([F:20])([F:19])[F:18])=[CH:13][CH:12]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 24386Thionyl ChlorideHCID 6736306N'-benzylidene-4-trifluoromethylbenzohydrazide

생성물 1

HCID 86593884N-benzylidene-4-trifluoromethylbenzenecarbohydrazonoyl chloride수율 59%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A mixture of N′-benzylidene-4-trifluoromethylbenzohydrazide (2.92 g), thionyl chloride (1.09 ml) and toluene (50 ml) was heated under reflux for 1 hr. After cooling, the reaction mixture was concentrated, and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=8:1, volume ratio) and recrystallized from hexane to give N-benzylidene-4-trifluoromethylbenzenecarbohydrazonoyl chloride (1.85 g, yield 59%) as pale-yellow plate crystals. melting point: 95–96° C.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux for 1 hr
  3. temperatureAfter cooling
  4. concentrationthe reaction mixture was concentrated
  5. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=8:1, volume ratio)
  6. customrecrystallized from hexane

출처 및 근거

ORD 기록
ord-6a103e3960444c18877c3231eeb865c1
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07223791B2

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