Ethyl Acetoacetate → HCID 178429264、化合物

HRID 27899ノート

反応式

HRID 27899 の反応式
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[N:8]=[N:9][C:10]([NH:13][NH2:14])=[CH:11][CH:12]=2)[CH2:3][CH2:2]1.[C:15](OCC)(=[O:20])[CH2:16][C:17]([CH3:19])=O.[OH-].[NH4+]>C(O)C>[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[N:8]=[N:9][C:10]([N:13]3[C:15]([OH:20])=[CH:16][C:17]([CH3:19])=[N:14]3)=[CH:11][CH:12]=2)[CH2:3][CH2:2]1

参加物

5

反応物 3

HCID 8868Ethyl AcetoacetateHCID 14923Ammonium HydroxideHCID 12603548HCID 12603548、化合物

生成物 1

HCID 178429264HCID 178429264、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 0.98 g (5 mmoles) of 3-morpholino-6-pyridazinyl-hydrazine, 0.65 g (5 mmoles) of ethyl acetoacetate and 15 ml of ethanol is stirred at reflux temperature for 3 hours. After cooling the mixture is stirred with 1 ml of concentrated aqueous ammonium hydroxide solution at room temperature for 4 hours and then left to stand overnight. The separated crystals are filtered, washed with water and recrystallized from ethanol. Yield: 0.5 g (39%); m.p.: 189°-192° C.

後処理

  1. temperatureat reflux temperature for 3 hours
  2. temperatureAfter cooling the mixture
  3. waitleft
  4. filtrationThe separated crystals are filtered
  5. washwashed with water
  6. customrecrystallized from ethanol

出典と根拠

ORDレコード
ord-f214f96a84e4413894227dd708debb19
出典データセット
uspto-grants-1980_09
特許番号
US04224325

反応ノート

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