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

HRID 1679760

반응식

HRID 1679760 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 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.

후처리

  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

출처 및 근거

ORD 기록
ord-caaeb24f5322455ca920835719684400
출처 데이터셋
uspto-grants-1978_03
특허 번호
US04081596

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