Potassium Hydroxide → Ethyl hydrogen diethylmalonate

HRID 1992100

반응식

HRID 1992100 반응식
[CH2:1]([O:3][C:4](=[O:15])[C:5]([CH2:13][CH3:14])([CH2:11][CH3:12])[C:6]([O:8]CC)=[O:7])[CH3:2].[OH-].[K+]>C(O)C>[CH2:1]([O:3][C:4]([C:5]([CH2:11][CH3:12])([CH2:13][CH3:14])[C:6]([OH:8])=[O:7])=[O:15])[CH3:2]

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 66165Diethyl diethylmalonate

생성물 1

HCID 13529198Ethyl hydrogen diethylmalonate수율 72.7%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of diethyl-malonic acid diethyl ester (3.0 g, 13.89 mmol) and potassium hydroxide (0.778 g, 13.89 mmol) in ethanol (50 ml) was stirred at room temperature for 18 hrs. The solvent was evaporated off and the residue was dissolved in water (20 ml) and extracted with dichloromethane (20 ml). This organic layer was discarded. The aqueous layer was then acidified with concentrated HCl and extracted with dichloromethane (3×20 ml). The combined organic layers were dried over magnesium sulfate and concentrated to give a colorless oil (1.9 g, 72%). 1H NMR (300 MHz, methanol-d4) δ 4.17 (m, 2H), 1.89 (m, 4H), 1.25 (m, 3H), 0.83 (m, 6H). ES-LCMS m/z 188 (M+H).

후처리

  1. customThe solvent was evaporated off
  2. dissolutionthe residue was dissolved in water (20 ml)
  3. extractionextracted with dichloromethane (20 ml)
  4. extractionextracted with dichloromethane (3×20 ml)
  5. dry with materialThe combined organic layers were dried over magnesium sulfate
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-54634cb66a2a469281e8da2ff6187d78
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07645771B2

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