HRID900421
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
3-Amino-5-(3-methoxyphenyl)-2-thiophenecarboxamide (0.5 g), trimethylsilylisocyanate (2 mL), dimethylformamide (2 mL) and dichloromethane were heated at reflux for 3 days. After cooling the solid was filtered off, suspended in dichloromethane (100 mL) and treated with boron tribromide (5 mL of a 1M solution in dichloromethane). After 3 days. methanol (50 mL) was added. After 1 h, the solvent was evaporated and the residue was triturated with 2M hydrochloric acid. The title urea was filtered off (0.35 g).
WORKUP
后处理
- temperatureat reflux for 3 days
- temperatureAfter cooling the solid
- filtrationwas filtered off
- additiontreated with boron tribromide (5 mL of a 1M solution in dichloromethane)
- additionmethanol (50 mL) was added
- waitAfter 1 h
- customthe solvent was evaporated
- customthe residue was triturated with 2M hydrochloric acid
- filtrationThe title urea was filtered off (0.35 g)