(4-bromo-2,6-dichlorophenyl)hydrazine → HCID 13118709、化合物

HRID 2418122ノート

反応式

HRID 2418122 の反応式
[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

  1. customThe butanol was evaporated off
  2. dissolutionthe oily residue was dissolved in 150 parts by volume of ether, and dry halogen chloride gas
  3. temperaturecooling
  4. customThe hydrochloride which had precipitated
  5. filtrationthe precipitate was filtered off with suction
  6. 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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