反应详情

To a stirring solution of glutaconic acid in DMF (0.1 M) at 0° C. was added NaH (1 eq). After 15 min, iodomethane (1.2 eq) was added, and the mixture was allowed to warm to room temperature overnight. The reaction was quenched with saturated ammonium chloride, and extracted with ethyl acetate. The organic phase was washed with water and brine, dried over magnesium sulfate, filtered and concentrated in vacuo. The residue was chromatographed (silica; 10% MeOH/CHCl3) to afford a colorless viscous oil. EI-MS m/z 143 (M−H)−

1. customThe reaction was quenched with saturated ammonium chloride
2. extractionextracted with ethyl acetate
3. washThe organic phase was washed with water and brine
4. dry with materialdried over magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was chromatographed (silica; 10% MeOH/CHCl3)
8. customto afford a colorless viscous oil