(4-bromo-2,6-dichlorophenyl)hydrazine → HCID 13118709、化合物
反応式
[Cl:1][C:2]1[CH:7]=[C:6]([Br:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[NH:10][NH2:11].C(O[CH:15]=[C:16]([C:23]#[N:24])[C:17]([O:19][CH2:20][CH:21]=[CH2:22])=[O:18])C>C(O)CCC>[NH2:24][C:23]1[N:10]([C:3]2[C:2]([Cl:1])=[CH:7][C:6]([Br:8])=[CH:5][C:4]=2[Cl:9])[N:11]=[CH:15][C:16]=1[C:17]([O:19][CH2:20][CH:21]=[CH2:22])=[O:18]参加物
4
実験手順
20.5 parts by weight of 2,6-dichloro-4-bromophenylhydrazine and 14.5 parts by weight of allyl ethoxymethylene-2-cyanoacetate in 100 parts by volume of n-butanol were refluxed for 4 hours. The butanol was evaporated off, the oily residue was dissolved in 150 parts by volume of ether, and dry halogen chloride gas was passed in, with ice-cooling. The hydrochloride which had precipitated was stirred with saturated sodium bicarbonate solution, and the precipitate was filtered off with suction and dried under reduced pressure to give 24.8 parts by weight of allyl 5-amino-1-(2,6-dichloro-4-bromophenyl)-pyrazole-4-carboxylate of melting point 85° C. (active ingredient No.6).
後処理
- customThe butanol was evaporated off
- dissolutionthe oily residue was dissolved in 150 parts by volume of ether, and dry halogen chloride gas
- temperaturecooling
- customThe hydrochloride which had precipitated
- filtrationthe precipitate was filtered off with suction
- customdried under reduced pressure
出典と根拠
- ORDレコード
- ord-8633e0185b894ba7a562047f7edce1d6
- 出典データセット
- uspto-grants-1984_09
- 特許番号
- US04472192
反応ノート
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