HRID32596

反应详情

EQUATION

反应方程式

HRID 32596 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

tert-Butyl 2-(aminocarbonyl)-3-furylcarbamate (Intermediate 82) (3.38 g) was stirred in DMF (25 mL) and DCM (25 mL) for 30 minutes. The solvent was removed and the crude product was heated at 80° C. in triethylorthoformate (20 mL) for 30 minutes. The mixture was cooled, poured into ether (100 mL) collected by filtration and washed with ether to afford a first crop of the title compound as a pale yellow solid (1.31 g, 65%). The filtrate was evaporated and triturated with EtOAc to afford a further crop (296 mg, 15%);

WORKUP

后处理

  1. customThe solvent was removed
  2. temperatureThe mixture was cooled
  3. additionpoured into ether (100 mL)
  4. filtrationcollected by filtration
  5. washwashed with ether