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

HRID 1709099노트

반응식

HRID 1709099 반응식
[Cl:1][C:2]1[CH:20]=[C:19]([Cl:21])[CH:18]=[CH:17][C:3]=1[O:4][C:5]1[CH:16]=[CH:15][C:8]([O:9][CH:10]([CH3:14])[C:11](Cl)=[O:12])=[CH:7][CH:6]=1.C([O-])(=O)CC([O-])=O.C(C(CC)(O[Mg+2])C)C.[C:37]([O:45][CH2:46][CH3:47])(=[O:44])[CH2:38][C:39]([O:41][CH2:42][CH3:43])=[O:40]>CCOCC>[CH2:42]([O:41][C:39](=[O:40])[CH:38]([C:11](=[O:12])[CH:10]([O:9][C:8]1[CH:15]=[CH:16][C:5]([O:4][C:3]2[CH:17]=[CH:18][C:19]([Cl:21])=[CH:20][C:2]=2[Cl:1])=[CH:6][CH:7]=1)[CH3:14])[C:37]([O:45][CH2:46][CH3:47])=[O:44])[CH3:43]

참가 물질

4

반응물 2

HCID 7761Diethyl MalonateHCID 129429952-[4-(2,4-Dichlorophenoxy)phenoxy]propanoyl chloride

생성물 1

HCID 23037017Diethyl-2-[4'-(2",4"-dichloro-phenoxy)-phenoxy]-propionyl-malonate수율 75%

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

A 50% etheral solution of 35 g of 2-[4'-(2",4"-dichloro-phenoxy)-phenoxy]-propionyl-chloride is added under stirring dropwise to a mixture of diethyl-ethoxy-magnesium-malonate prepared from 17.6 g of diethyl malonate and 50 ml of ether. The addition of the acid chloride having been completed the reaction mixture is heated to boiling for an hour, cooled to room temperature and washed successively with 100 ml of 5% sulfuric acid, 100 ml of a 6% sodium bicarbonate solution and 100 ml of water. The etheral phase is evaporated, the excess of the malonic acid ester is distilled off, the residue is admixed with 100 ml of benzene, subjected to chromatography on a silica column and eluted with 50 ml of benzene. The united eluates are evaporated. Thus 35 g of the desired compound are obtained in the form of a slowly solidifying product. Mp.: 46°-50° C. Yield 75%.

후처리

  1. temperatureis heated
  2. waitto boiling for an hour
  3. washwashed successively with 100 ml of 5% sulfuric acid, 100 ml of a 6% sodium bicarbonate solution and 100 ml of water
  4. customThe etheral phase is evaporated
  5. distillationthe excess of the malonic acid ester is distilled off
  6. washeluted with 50 ml of benzene
  7. customThe united eluates are evaporated

출처 및 근거

ORD 기록
ord-9592c9050e74495ba940061c3fce8a6d
출처 데이터셋
uspto-grants-1990_08
특허 번호
US04948420

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