Diethyl Malonate → Diethyl 2-cyclohexylmethylmalonate

HRID 1248191노트

반응식

HRID 1248191 반응식
[C:1]([O:9][CH2:10][CH3:11])(=[O:8])[CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].[CH:12]1([CH2:18]Br)[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1>[O-]CC.[Na+]>[CH2:10]([O:9][C:1](=[O:8])[CH:2]([CH2:18][CH:12]1[CH2:17][CH2:16][CH2:15][CH2:14][CH2:13]1)[C:3]([O:5][CH2:6][CH3:7])=[O:4])[CH3:11]

참가 물질

4

반응물 2

HCID 7761Diethyl MalonateHCID 137636Cyclohexane, (bromomethyl)-

생성물 1

HCID 599487Diethyl 2-cyclohexylmethylmalonate수율 66.4%

시약·촉매·용매 1

HCID 2723922Sodium ethoxide용매

실험 절차

Diethyl malonate (16.0 g) was added to a freshly prepared solution of sodium ethoxide (from 2.3 g of sodium in 150 ml of absolute ethanol), followed by 17.7 g of cyclohexylmethyl bromide. The mixture was heated under reflux for four hours and evaporated to dryness. The resulting mixture was treated with water, extracted with ethyl acetate and the extracts washed with water, brine and dried (MgSO4). Evaporation gave an oil which was distilled in vacuo to give 17 g of diethyl(cyclohexylmethyl)malonate (b.p. 104°-107° C. at 0.2 mm Hg).

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for four hours
  3. customevaporated to dryness
  4. additionThe resulting mixture was treated with water
  5. extractionextracted with ethyl acetate
  6. washthe extracts washed with water, brine
  7. dry with materialdried (MgSO4)
  8. customEvaporation
  9. customgave an oil which
  10. distillationwas distilled in vacuo

출처 및 근거

ORD 기록
ord-53f0910570d849d6a8ea5ee573fe74e8
출처 데이터셋
uspto-grants-1985_06
특허 번호
US04522948

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