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

HRID 1197270

Reaktionsgleichung

Reaktionsgleichung von HRID 1197270
[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]

Komponenten

6

Versuchsvorschrift

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.

Aufarbeitung

  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

Quellen und Nachweise

ORD-Eintrag
ord-38a1297a41124d359011cfaf416cacc4
Quelldatensatz
uspto-grants-1992_05
Patentnummer
US05117057

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