Oxalyl chloride → N'-t-butyl-N-benzoyl-N'-(beta-trifluoromethylcrotonyl)hydrazine

HRID 1197270노트

반응식

HRID 1197270 반응식
[C:1]([NH:5][NH:6][C:7](=[O:14])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].[F:15][C:16]([F:24])([F:23])/[C:17](/[CH3:22])=[CH:18]\[C:19](Cl)=[O:20].C(Cl)(=O)C(Cl)=O.FC(F)(F)/C(/C)=C\C(O)=O>C1(C)C=CC=CC=1>[C:1]([N:5]([C:19](=[O:20])/[CH:18]=[C:17](\[C:16]([F:24])([F:23])[F:15])/[CH3:22])[NH:6][C:7](=[O:14])[C:8]1[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=1)([CH3:4])([CH3:2])[CH3:3]

참가 물질

6

반응물 4

HCID 65578Oxalyl chlorideHCID 299436N'-tert-butylbenzohydrazideHCID 57088354,4,4-Trifluoro-3-methyl-2-butenoic acidHCID 86745869beta-Trifluoromethylcrotonyl chloride

생성물 1

HCID 70294050N'-t-butyl-N-benzoyl-N'-(beta-trifluoromethylcrotonyl)hydrazine

시약·촉매·용매 1

HCID 1140Toluene용매2회

실험 절차

N'-t-butyl-N-benzoylhydrazine (1.0 g,) in 2 ml toluene was added dropwise to a solution of beta-trifluoromethylcrotonyl chloride (prepared by addition of oxalyl chloride (1.3 g) to a solution of 1.5 g beta-trifluoromethylcrotonic acid in 5 ml toluene at 23° C.). After 30 min. at 23° C., the reaction mixture was partitioned between saturated aqueous sodium bicarbonate (20 ml) and ether (20 ml). The ether layer was evaporated under reduced pressure to about 10 ml and the excess hydrazine was removed by filtration. The filtrate was evaporated to give N'-t-butyl-N-benzoyl-N'-(beta-trifluoromethylcrotonyl)hydrazine as a colorless oil.

후처리

  1. customthe reaction mixture was partitioned between saturated aqueous sodium bicarbonate (20 ml) and ether (20 ml)
  2. customThe ether layer was evaporated under reduced pressure to about 10 ml
  3. customthe excess hydrazine was removed by filtration
  4. customThe filtrate was evaporated

출처 및 근거

ORD 기록
ord-38a1297a41124d359011cfaf416cacc4
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05117057

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