HRID900421

反应详情

EQUATION

反应方程式

HRID 900421 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureat reflux for 3 days
  2. temperatureAfter cooling the solid
  3. filtrationwas filtered off
  4. additiontreated with boron tribromide (5 mL of a 1M solution in dichloromethane)
  5. additionmethanol (50 mL) was added
  6. waitAfter 1 h
  7. customthe solvent was evaporated
  8. customthe residue was triturated with 2M hydrochloric acid
  9. filtrationThe title urea was filtered off (0.35 g)