Hydrazine hydrate (1:1) → 4-Cyano-5-hydrazino-1-(2,4-dichlorophenyl)-pyrazole
反応式
Br[C:2]1[N:6]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][C:8]=2[Cl:14])[N:5]=[CH:4][C:3]=1[C:15]#[N:16].O.[NH2:18][NH2:19]>O1CCOCC1>[C:15]([C:3]1[CH:4]=[N:5][N:6]([C:7]2[CH:12]=[CH:11][C:10]([Cl:13])=[CH:9][C:8]=2[Cl:14])[C:2]=1[NH:18][NH2:19])#[N:16]参加物
4
実験手順
6.4 g (0.02 mol) of 5-bromo-4-cyano-1-(2,4-dichlorophenyl)-pyrazole and 15 g (0.2 mol) of hydrazine hydrate in 80 ml of dioxane are stirred at the reflux temperature for 20 hours, the mixture is then concentrated under reduced pressure and the residue is stirred with water, filtered off with suction and recrystallized twice from ethanol. 2.1 g (40% of theory) of 4-cyano-5-hydrazino-1-(2,4-dichlorophenyl)-pyrazole of melting point 199° C.-204° C. are obtained.
後処理
- concentrationthe mixture is then concentrated under reduced pressure
- filtrationfiltered off with suction
- customrecrystallized twice from ethanol
出典と根拠
- ORDレコード
- ord-8094ee253dbb4e3b86920b9c8f629b1c
- 出典データセット
- uspto-grants-1988_09
- 特許番号
- US04770688
反応ノート
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