Hydrazine hydrate (1:1) → 6-(4-benzylamino-3-hydroxy-phenyl)-5-methyl-4,5-dihydro-2H-pyridazin-3-one

HRID 1619966ノート

反応式

HRID 1619966 の反応式
O.[NH2:2][NH2:3].[CH2:4]([NH:11][C:12]1[CH:17]=[CH:16][C:15]([C:18](=O)[CH:19]([CH3:24])[CH2:20][C:21](O)=[O:22])=[CH:14][C:13]=1[OH:26])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>C(O)(=O)C>[CH2:4]([NH:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[CH:19]([CH3:24])[CH2:20][C:21](=[O:22])[NH:2][N:3]=2)=[CH:14][C:13]=1[OH:26])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 674661774-(4-Benzylamino-3-hydroxy-phenyl)-3-methyl-4-oxo-butyric acid

生成物 1

HCID 674671166-(4-benzylamino-3-hydroxy-phenyl)-5-methyl-4,5-dihydro-2H-pyridazin-3-one

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
110 °C

実験手順

While cooling with the ice bath 69.9 ml (1396 mmol) hydrazine hydrate are added dropwise to 220 ml glacial acetic acid, then 54.7 g (175 mmol) 4-(4-benzylamino-3-hydroxy-phenyl)-3-methyl-4-oxo-butyric acid are added and the mixture is stirred for 1.5 h at 110° C. Then the mixture is cooled somewhat and poured onto ice water, the precipitated product is suction filtered, washed first with copious amounts of water, then with a little acetone and then dried in the vacuum dryer.

後処理

  1. temperatureThen the mixture is cooled somewhat
  2. additionpoured onto ice water
  3. filtrationfiltered
  4. washwashed first with copious amounts of water
  5. dry with materialwith a little acetone and then dried in the vacuum dryer

出典と根拠

ORDレコード
ord-01efdea66a83440794839b1af17bcc3a
出典データセット
uspto-grants-2014_07
特許番号
US08772323B2

反応ノート

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