反应详情

温度

50 °C

0.70 g (2 mmol) of the product of Example 15 was dissolved in benzene dehydrated over calcium hydride, 0.3 ml (5 mmol) of methyl isocyanate was added and the reaction mixture was stirred at 50° C. for 4 hours. The crystals formed after coling were filtered, washed with 3×3 ml of benzene, then triturated with 20 ml of hot benzene. The hot mixture was filtered, the precipitate was washed with 3×3 ml of benzene and dried to give 0.65 g (79.6%) of the aimed product, m.p.: 168°-170° C. (decomp.).

1. additionwas added
2. customThe crystals formed
3. filtrationafter coling were filtered
4. washwashed with 3×3 ml of benzene
5. customtriturated with 20 ml of hot benzene
6. filtrationThe hot mixture was filtered
7. washthe precipitate was washed with 3×3 ml of benzene
8. customdried