Ethyl Acetoacetate → HCID 20361945、化合物

HRID 1679754ノート

反応式

HRID 1679754 の反応式
C(O[C:4](=[O:9])[CH2:5][C:6]([CH3:8])=O)C.[CH3:10][CH:11]([NH:19][NH2:20])[C:12]1[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=1>C(O)C>[CH3:8][C:6]1[NH:20][N:19]([CH:11]([CH3:10])[C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=2)[C:4](=[O:9])[CH:5]=1

参加物

4

反応物 2

HCID 8868Ethyl AcetoacetateHCID 12489385HCID 12489385、化合物

生成物 1

HCID 20361945HCID 20361945、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

26 g of acetoacetic acid ethyl ester were dissolved in 20 ml of absolute ethanol. 30.0 g of α-methyl-4-methylbenzylhydrazine in a little absolute ethanol were slowly added to this solution under nitrogen. After the exothermic reaction had subsided, the mixture was heated for 2 hours under reflux. On cooling, the crude product crystallized out and was purified by recrystallization from methanol. Melting point 144°-146° C; yield 28 g (65% of theory).

後処理

  1. customAfter the exothermic reaction
  2. temperaturethe mixture was heated for 2 hours
  3. temperatureunder reflux
  4. temperatureOn cooling
  5. customthe crude product crystallized out
  6. customwas purified by recrystallization from methanol

出典と根拠

ORDレコード
ord-e25f2ff490944f07953391359dbcbda2
出典データセット
uspto-grants-1978_03
特許番号
US04081596

反応ノート

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