Benzene → Ethyl 2-[2-(2,4,6-trichlorophenyl)hydrazinylidene]butanoate

HRID 435581

반응식

HRID 435581 반응식
O=[C:2]([CH2:8][CH3:9])[C:3]([O:5][CH2:6][CH3:7])=[O:4].[Cl:10][C:11]1[CH:16]=[C:15]([Cl:17])[CH:14]=[C:13]([Cl:18])[C:12]=1[NH:19][NH2:20].C1C=CC=CC=1>O>[Cl:10][C:11]1[CH:16]=[C:15]([Cl:17])[CH:14]=[C:13]([Cl:18])[C:12]=1[NH:19][N:20]=[C:2]([CH2:8][CH3:9])[C:3]([O:5][CH2:6][CH3:7])=[O:4]

참가 물질

5

반응물 3

HCID 241BenzeneHCID 79234(2,4,6-Trichlorophenyl)hydrazineHCID 85195ethyl acetoacetate, sodium salt

생성물 1

HCID 71365097Ethyl 2-[2-(2,4,6-trichlorophenyl)hydrazinylidene]butanoate

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

A reaction mixture consisting of 11 g. (0.085 mole) ethyl 2-oxobutyrate, 17 g. (0.077 mole) (2,4,6-trichlorophenyl)hydrazine, and 200 ml. benzene was heated at the reflux temperature with a Dean and Stark water trap attached to the reaction vessel. When all the water produced by the reaction had been removed, the benzene was removed by evaporation under reduced pressure. The oily residue that remained was dissolved in hot technical hexane, and this solution was allowed to cool. Crystals of the desired product separated and 15.2 g. were recovered. Recrystallization from methanol gave an analytical sample of ethyl 2-oxobutyrate 2-(2,4,6-trichlorophenyl)hydrazone having a melting point at 97° to 99° C.

후처리

  1. customhad been removed
  2. customthe benzene was removed by evaporation under reduced pressure
  3. dissolutionThe oily residue that remained was dissolved in hot technical hexane
  4. temperatureto cool
  5. customCrystals of the desired product separated
  6. customwere recovered
  7. customRecrystallization from methanol

출처 및 근거

ORD 기록
ord-c1da97d1c7cb4774abed18b13dd1c226
출처 데이터셋
uspto-grants-1977_02
특허 번호
US04006132

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