反应详情

温度

0 °C

To a solution of 2-chloro-N-cyclopropyl-acetamide (58.1 g, 0.435 mol) in dichloromethane (700 ml) at 0° C. is added thiolactic acid (49.65 g, 0.652 mol). The mixture is stirred at 0° C. for 5 minutes, then TEA (88.0 g, 0.870 mol) is added very slowly (exothermic reaction). The mixture is stirred at 0° C. for 2 hours, then poured over 700 ml of water with stirring. The aqueous layer is acidified to pH2 with 5 N HCl, and the layers are shaken and separated. The aqueous layer is extracted with dichloromethane (2×400 ml). The combined organic layers are washed with brine, then dried (anhydrous magnesium sulfate), filtered, and concentrated to give the title compound as a yellow-orange solid (74.5 g, 99%). Mass (m/z): 174.1 (M++1).

1. custom(exothermic reaction)
2. stirringThe mixture is stirred at 0° C. for 2 hours
3. stirringwith stirring
4. stirringthe layers are shaken
5. customseparated
6. extractionThe aqueous layer is extracted with dichloromethane (2×400 ml)
7. washThe combined organic layers are washed with brine
8. dry with materialdried (anhydrous magnesium sulfate)
9. filtrationfiltered
10. concentrationconcentrated