Diethyl Malonate → Diethyl 2-cyclohexylmethylmalonate

HRID 1060731노트

반응식

HRID 1060731 반응식
[Na].[C:2]([O:10][CH2:11][CH3:12])(=[O:9])[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[CH:13]1([CH2:19]Br)[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1>C(O)C>[CH:13]1([CH2:19][CH:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])[C:2]([O:10][CH2:11][CH3:12])=[O:9])[CH2:18][CH2:17][CH2:16][CH2:15][CH2:14]1

참가 물질

5

반응물 3

HCID 7761Diethyl MalonateHCID 137636Cyclohexane, (bromomethyl)-HCID 5360545Sodium

생성물 1

HCID 599487Diethyl 2-cyclohexylmethylmalonate

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
70 °C

실험 절차

A solution comprised of sodium (6.9 g, 0.3 mmol) in ethanol (250 mL) was treated sequentially with diethyl malonate (53.127 g, 0.3 mol) and then cyclohexylmethyl bromide (46 mL, 0.33 mol) at ambient temperature. The mixture was heated to 70° C. and stirred for approximately 12 hours. The mixture was cooled and solvent was removed by evaporation. The residue was diluted with ice water and the dilution was extracted with ethyl acetate (4×). The combined extracts were washed with water (4×) and brine, dried (MgSO4) and concentrated to provide diethyl 2-cyclohexylmethylmalonate.

후처리

  1. customat ambient temperature
  2. temperatureThe mixture was cooled
  3. customsolvent was removed by evaporation
  4. additionThe residue was diluted with ice water
  5. extractionthe dilution was extracted with ethyl acetate (4×)
  6. washThe combined extracts were washed with water (4×) and brine
  7. dry with materialdried (MgSO4)
  8. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f9599f35ecd5494fa60a52163df24231
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525036B2

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