反应详情

To a mixture of 0.50 g of 1,2-dimethyl-3-nitroisothiourea and 10 ml of pyridine was dropwise added 1.03 g of acetic anhydride at room temperature. The mixture was stirred at room temperature for 1 hour, and then poured onto 150 ml of 2N hydrochloric acid followed by extraction with 100 ml of chloroform. The chloroform layer was washed with 50 ml of 2N hydrochloric acid and then concentrated to give 0.60 g of 1-acetyl-1,2-dimethyl-3-nitroisothiourea as pale yellow liquid. NMR (CDCl3):2.23(3H, s), 2.52(3H, s), 3.17(3H, s).

1. customat room temperature
2. extractionfollowed by extraction with 100 ml of chloroform
3. washThe chloroform layer was washed with 50 ml of 2N hydrochloric acid
4. concentrationconcentrated