HRID36866

反应详情

EQUATION

反应方程式

HRID 36866 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

4.8 g (0.12 mol) of a 60% sodium hydride solution are added, at 0° C., under argon, and in portions, to a solution of 34 g (0.11 mol) of ethyl 2-[[(1,1-dimethylethoxy)carbonyl]amino]-3-nitrobenzoate in 100 ml of dimethylformamide. The mixture is left stirring for 20 minutes at 0° C. 55.9 g (0.33 mol) of 2-iodopropane are then added and the mixture is heated at 80° C. for 4 hours and then at room temperature for 48 hours. Hydrolysis is carried out by adding water and extraction is carried out 3 times with ethyl acetate. The organic phase is collected and washed successively with water and with a saturated sodium chloride solution. It is dried and evaporated.

WORKUP

后处理

  1. waitThe mixture is left
  2. temperaturethe mixture is heated at 80° C. for 4 hours
  3. waitat room temperature for 48 hours
  4. customHydrolysis
  5. additionby adding
  6. extractionwater and extraction
  7. customThe organic phase is collected
  8. washwashed successively with water and with a saturated sodium chloride solution
  9. customIt is dried
  10. customevaporated