Potassium Hydroxide → Ethyl hydrogen diethylmalonate

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).

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

ORDレコード

ord-54634cb66a2a469281e8da2ff6187d78

出典データセット

uspto-grants-2010_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07645771B2