(3-(Trifluoromethyl)phenyl)hydrazine → 4,5-Dibromo-2-[3-(trifluoromethyl)phenyl]pyridazin-3(2H)-one

HRID 1902832ノート

反応式

HRID 1902832 の反応式
[C:1](O)(=O)/[C:2](=[C:4](\[CH:6]=[O:7])/[Br:5])/[Br:3].[F:10][C:11]([F:21])([F:20])[C:12]1[CH:13]=[C:14]([NH:18][NH2:19])[CH:15]=[CH:16][CH:17]=1>C(O)C>[F:10][C:11]([F:20])([F:21])[C:12]1[CH:13]=[C:14]([N:18]2[C:6](=[O:7])[C:4]([Br:5])=[C:2]([Br:3])[CH:1]=[N:19]2)[CH:15]=[CH:16][CH:17]=1

参加物

4

反応物 2

HCID 98650(3-(Trifluoromethyl)phenyl)hydrazineHCID 3033972Mucobromic Acid

生成物 1

HCID 167793014,5-Dibromo-2-[3-(trifluoromethyl)phenyl]pyridazin-3(2H)-one収率 68.9%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 21.4 grams of mucobromic acid and 13.3 grams of 3-trifluoromethylphenyl hydrazine in 60 milliliters of ethanol was stirred for about 10 minutes. The ethanol was removed by evaporation under reduced pressure, and then 40 milliliters each of glacial acetic acid and acetic anhydride were added to the reaction vessel. The acidic reaction mixture was heated at reflux for 4 hours. The reaction solvent was removed by evaporation under reduced pressure whereupon a solid precipitate formed. The solid was purified by recrystallization from ethanol. A yield of 20.7 grams of 1-(3-trifluoromethylphenyl)-4,5-dibromo-1,6-dihydro-6-oxopyridazine was obtained.

後処理

  1. customThe ethanol was removed by evaporation under reduced pressure
  2. addition40 milliliters each of glacial acetic acid and acetic anhydride were added to the reaction vessel
  3. temperatureThe acidic reaction mixture was heated
  4. temperatureat reflux for 4 hours
  5. customThe reaction solvent was removed by evaporation under reduced pressure whereupon a solid precipitate
  6. customformed
  7. customThe solid was purified by recrystallization from ethanol

出典と根拠

ORDレコード
ord-4912cb79dc0b4c9dbcf5dc2e40300929
出典データセット
uspto-grants-1982_12
特許番号
US04366155

反応ノート

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