Diethyl-2-chloro-propionyl-malonate → Diethyl-2-[4'-(2",4"-dichloro-phenoxy)-phenoxy]-propionyl-malonate

HRID 1709101노트

반응식

HRID 1709101 반응식
[Na].[Cl:2][C:3]1[CH:16]=[C:15]([Cl:17])[CH:14]=[CH:13][C:4]=1[O:5][C:6]1[CH:11]=[CH:10][C:9]([O-:12])=[CH:8][CH:7]=1.[CH2:18]([O:20][C:21](=[O:33])[CH:22]([C:28](=[O:32])[CH:29](Cl)[CH3:30])[C:23]([O:25][CH2:26][CH3:27])=[O:24])[CH3:19]>CS(C)=O>[CH2:26]([O:25][C:23](=[O:24])[CH:22]([C:28](=[O:32])[CH:29]([O:12][C:9]1[CH:8]=[CH:7][C:6]([O:5][C:4]2[CH:13]=[CH:14][C:15]([Cl:17])=[CH:16][C:3]=2[Cl:2])=[CH:11][CH:10]=1)[CH3:30])[C:21]([O:20][CH2:18][CH3:19])=[O:33])[CH3:27]

참가 물질

4

반응물 2

HCID 19765057Diethyl-2-chloro-propionyl-malonateHCID 86744142Sodium 4-(2',4'-dichloro-phenoxy)-phenolate

생성물 1

HCID 23037017Diethyl-2-[4'-(2",4"-dichloro-phenoxy)-phenoxy]-propionyl-malonate수율 63.9%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

반응 조건

온도
60 °C

실험 절차

27.7 g of sodium-4-(2',4'-dichloro-phenoxy)-phenolate and 25.1 g of diethyl-2-chloro-propionyl-malonate are dissolved in 150 ml of dimethyl sulfoxide and the reaction mixture is stirred at 60° C. for 48 hours under stirring. The reaction mixture is filtered and the filtrate is evaporated. The residue is dissolved in 100 ml of benzene and washed successively with 100 ml of a saturated aqueous sodium hydrogen carbonate solution and water. The benzene solution is evaporated. Thus 30 g of the desired compound are obtained, yield 61%.

후처리

  1. stirringunder stirring
  2. filtrationThe reaction mixture is filtered
  3. customthe filtrate is evaporated
  4. dissolutionThe residue is dissolved in 100 ml of benzene
  5. washwashed successively with 100 ml of a saturated aqueous sodium hydrogen carbonate solution and water
  6. customThe benzene solution is evaporated

출처 및 근거

ORD 기록
ord-41bffb4b3a5a4b44a31d7fde63e87897
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04948420

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