Acetone → 1,3-Dimethyl 2-(propan-2-ylidene)propanedioate

HRID 1974438노트

반응식

HRID 1974438 반응식
[C:1]([O:8][CH3:9])(=[O:7])[CH2:2][C:3]([O:5][CH3:6])=[O:4].[CH3:10][C:11]([CH3:13])=O.O>C(OC(=O)C)(=O)C.[Cl-].[Zn+2].[Cl-]>[C:11](=[C:2]([C:1]([O:8][CH3:9])=[O:7])[C:3]([O:5][CH3:6])=[O:4])([CH3:13])[CH3:10]

참가 물질

6

반응물 3

HCID 180AcetoneHCID 962WaterHCID 7943Dimethyl malonate

생성물 1

HCID 51620841,3-Dimethyl 2-(propan-2-ylidene)propanedioate

시약·촉매·용매 2

HCID 3007855Zincchloride촉매HCID 7918Acetic Anhydride용매

실험 절차

A solution of 51 grams (0.39 mol) of dimethyl malonate, 30 grams of acetone, and 2.5 grams of zinc chloride in 50 mL of acetic anhydride was refluxed with stirring for 24 hours. The solution was poured into ice and water, then extracted with 200 mL of dichloromethane. The organic phase was washed 2×150 mL water, dried over sodium sulfate and concentrated to a brown oil. After two distillations the 41 gram fraction collected at 25°-34° C. (0.1 mm Hg) gave satisfactory analytical for dimethyl isopropylidenemalonate.

후처리

  1. extractionextracted with 200 mL of dichloromethane
  2. washThe organic phase was washed 2×150 mL water
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated to a brown oil
  5. distillationAfter two distillations the 41 gram fraction collected at 25°-34° C. (0.1 mm Hg)

출처 및 근거

ORD 기록
ord-8ec5d3ea36424554b5aca9e8f7f9ab82
출처 데이터셋
uspto-grants-1994_02
특허 번호
US05283165

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