反应详情

温度

120 °C

To a solution of 1,3 dichloroacetone (0.42 g, 3.26 mmol) in toluene (5 mL) was added 3-hydroxythiobenzamide (0.25 g, 1.63 mmol) and the reaction mixture was heated at 120° C. for 1 h. After completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness, added water and extracted with EtOAc (×3). The combined organics was washed with water, brine, dried (Na2SO4), filtered and concentrated. The crude residue was purified over silica gel (230-400 M, 10% EtOAc-Hexane) to get the desired product (0.14 g, 38%).

1. customAfter completion of the reaction mixture (TLC monitoring), the reaction mixture was evaporated to dryness
2. additionadded water
3. extractionextracted with EtOAc (×3)
4. washThe combined organics was washed with water, brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. customThe crude residue was purified over silica gel (230-400 M, 10% EtOAc-Hexane)