反应详情

Thiophosgene (10.9 mls, 0.14 moles) is added dropwise to a well stirred mixture of undecylamine (49.9 g, 0.29 moles) and water (400 mls). The mixture is heated to reflux following the addition. After 45 minutes the mixture is allowed to cool while potassium carbonate (20.0 g, 0.14 moles) is added in portions, and is then reheated to reflux. After three hours the mixture is cooled and the product is filtered off, triturated in 2N HCl, refiltered, rinsed with water, and dried. Recrystallization from ethylacetate gave the product (32.7 g) mp 70°-72° C.

1. temperatureThe mixture is heated
2. temperatureto reflux
3. additionthe addition
4. additionis added in portions
5. temperatureto reflux
6. temperatureAfter three hours the mixture is cooled
7. filtrationthe product is filtered off
8. customtriturated in 2N HCl
9. washrinsed with water
10. customdried
11. customRecrystallization from ethylacetate