HRID1927569

反应详情

EQUATION

反应方程式

HRID 1927569 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 204 mg of Na2SO3 and 409 mg of NaHCO3 in 4 ml H2O is heated to 75° and treated portionwise with 0.5 g of 2-tert-butyl-6-chloro-benzooxazole-7-sulfonyl chloride (US 2007/0249672 page 9). A mixture obtained is heated at 75° for 2 hours and 4 ml of EtOH are added followed by 0.11 ml of iodomethane. A mixture obtained is heated at 90° overnight and allowed to cool to rt. A mixture obtained is extracted with 3×30 ml of EtOAc and the combined organic extracts obtained are washed with brine, dried over MgSO4 and solvent is evaporated. The title compound is obtained.

WORKUP

后处理

  1. customA mixture obtained
  2. temperatureis heated at 75° for 2 hours
  3. customA mixture obtained
  4. temperatureis heated at 90° overnight
  5. customA mixture obtained
  6. extractionis extracted with 3×30 ml of EtOAc
  7. customthe combined organic extracts obtained
  8. washare washed with brine
  9. dry with materialdried over MgSO4 and solvent
  10. customis evaporated