Ethanol → 4-Chloro-2-(4-chlorophenyl)-5-hydroxypyridazin-3(2H)-one

HRID 1165425

反応式

HRID 1165425 の反応式
[OH-].[K+].[Cl:3][C:4]1[C:5](=[O:18])[N:6]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)[N:7]=[CH:8][C:9]=1Cl.C([OH:21])C>O>[Cl:3][C:4]1[C:5](=[O:18])[N:6]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)[N:7]=[CH:8][C:9]=1[OH:21]

参加物

5

反応物 3

HCID 702EthanolHCID 14797Potassium HydroxideHCID 7794024,5-Dichloro-2-(4-chlorophenyl)-3(2H)-pyridazinone

生成物 1

HCID 546974414-Chloro-2-(4-chlorophenyl)-5-hydroxypyridazin-3(2H)-one

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

In 140 ml of water was dissolved 18.3 g (0.28 mol) of potassium hydroxide, and thereto were added 25.6 g (0.093 mol) of 4,5-dichloro-2-(4-chlorophenyl)-3(2H)-pyridazinone and 140 ml of ethanol. The reaction mixture was refluxed for 6 hours. After allowing to cool, ethanol was distilled off from the mixture under reduced pressure and then 300 of water was added to the mixture. Insoluble matter was removed by filtration and filtrate was acidified with hydrochloric acid. The solid thus precipitated was taken out by filtration, washed with water, and recrystallized from ethanol to give 11.1 g of the intended compound having melting point (hereinafter referred to as "m.p.") of 270°-271° C.

後処理

  1. temperatureThe reaction mixture was refluxed for 6 hours
  2. temperatureto cool
  3. distillationethanol was distilled off from the mixture under reduced pressure
  4. addition300 of water was added to the mixture
  5. customInsoluble matter was removed by filtration and filtrate
  6. customThe solid thus precipitated
  7. filtrationwas taken out by filtration
  8. washwashed with water
  9. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-31fcf984d4d147f0a84abe9d0f46f7ec
出典データセット
uspto-grants-1990_03
特許番号
US04910201

関連ノート

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