反应详情

To a stirred solution of 1,3-dichloroacetone (6.85 g, 54 mmol) and ethyl 3-mercaptopropionate (13.9 mL, 108 mmol) in anhydrous tetrahydrofuran (150 mL) was dropwise added triethylamine (15.0 mL, 108 mmol) at 0° C. and stirred at room temperature for 24 h. The solvent was evaporated and the residue was partitioned between water and ethyl acetate. The ethyl acetate phase was washed with 5% hydrochloric acid and then brine, dried over sodium sulfate, and concentrated to dryness, affording 17.4 g of the crude 1,3-bis(2-ethoxycarbonylethylthio)acetone.

1. customat 0° C.
2. customThe solvent was evaporated
3. customthe residue was partitioned between water and ethyl acetate
4. washThe ethyl acetate phase was washed with 5% hydrochloric acid
5. dry with materialbrine, dried over sodium sulfate
6. concentrationconcentrated to dryness