Ethyl acetylphenylacetate → 3-Methyl-4-phenyl-1-(alpha-methyl-3,4-dichlorobenzyl)-5-pyrazolone

HRID 1679760

反応式

HRID 1679760 の反応式
C(O[C:4](=[O:15])[CH:5]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:6]([CH3:8])=O)C.[CH3:16][CH:17]([NH:26][NH2:27])[C:18]1[CH:23]=[CH:22][C:21]([Cl:24])=[C:20]([Cl:25])[CH:19]=1>C(O)C>[CH3:8][C:6]1[NH:27][N:26]([CH:17]([CH3:16])[C:18]2[CH:23]=[CH:22][C:21]([Cl:24])=[C:20]([Cl:25])[CH:19]=2)[C:4](=[O:15])[C:5]=1[C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

参加物

4

反応物 2

HCID 95389Ethyl acetylphenylacetateHCID 3016950(1-(3,4-Dichlorophenyl)ethyl)hydrazine

生成物 1

HCID 203358943-Methyl-4-phenyl-1-(alpha-methyl-3,4-dichlorobenzyl)-5-pyrazolone

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

20.6 g of α-phenylacetoacetic acid ethyl ester were added dropwise under nitrogen to a solution of 20.5 g (0.1 mol) of α-methyl-3,4-dichlorobenzylhydrazine in 20 ml of absolute ethanol, during which the temperature of the reaction mixture rose to 55° C. After heating the reaction solution for 2 hours under reflux, the reaction product crystallized out on cooling the reaction mixture. The crystals were filtered off, rinsed with ether and recrystallized from an ethanol/dimethyl formamide mixture.

後処理

  1. customrose to 55° C
  2. temperatureAfter heating the reaction solution for 2 hours
  3. temperatureunder reflux
  4. customthe reaction product crystallized out
  5. temperatureon cooling the reaction mixture
  6. filtrationThe crystals were filtered off
  7. washrinsed with ether
  8. customrecrystallized from an ethanol/dimethyl formamide mixture

出典と根拠

ORDレコード
ord-caaeb24f5322455ca920835719684400
出典データセット
uspto-grants-1978_03
特許番号
US04081596

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