Methylhydrazine → Ethyl 3-difluoromethyl-1-methyl-4-pyrazole carboxylate
反応式
F[B-](F)(F)F.[F:6][CH:7]([F:22])[C:8](=[N+:19](C)C)/[C:9](/[C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:10]\[N:11](C)[CH3:12].CNN>C(#N)C>[F:6][CH:7]([F:22])[C:8]1[C:9]([C:14]([O:16][CH2:17][CH3:18])=[O:15])=[CH:10][N:11]([CH3:12])[N:19]=1参加物
4
実験手順
10.0 g (30 mmol) of N-[(2E)-1-(difluoromethyl)-3-(dimethylamino)-2-(ethoxycarbonyl)prop-2-en-1-ylidene]-N-methylmethanaminium tetrafluoroborate were dissolved in 50 ml of acetonitrile and admixed with 2.3 g of methylhydrazine. After stirring at RT for 2 h, the acetonitrile was removed completely under reduced pressure. Distillation under reduced pressure or crystallization from n-hexane afforded 5.3 g (86% of theory) of the product having an m.p. of 63-65° C.
後処理
- customthe acetonitrile was removed completely under reduced pressure
- distillationDistillation
- customunder reduced pressure or crystallization from n-hexane
- customafforded 5.3 g (86% of theory) of the product
出典と根拠
- ORDレコード
- ord-7fdf5d01d81a4c53b28ce68e38b82729
- 出典データセット
- uspto-grants-2011_05
- 特許番号
- US07939673B2
反応ノート
読み込み中…