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

HRID 1076705

반응식

HRID 1076705 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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 two 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/dimethylformamide mixture.

후처리

  1. customrose to 55°C
  2. temperatureAfter heating the reaction solution for two 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/dimethylformamide mixture

출처 및 근거

ORD 기록
ord-ad570870fa5f439fb5f182e25e8fff86
출처 데이터셋
uspto-grants-1976_05
특허 번호
US03957814

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