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

HRID 849770ノート

反応式

HRID 849770 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a0ec4bd5c3bd41b99ae4fbc230312fe8
出典データセット
uspto-grants-2000_01
特許番号
US06013836

反応ノート

読み込み中…