HRID1013383

反应详情

EQUATION

反应方程式

HRID 1013383 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the product from step k) (110 mg, 0.42 mmol) in AcOH (1 ml) and CHCl3 (1 ml) was treated with hydroquinone (5 mg) and NBS (77.8 mg, 0.437 mmol) at 40° C. for 3 hours in the dark. Next, the reaction mixture was carefully quenched with sat. NaHCO3 (5 ml) and extracted with EtOAc (3×20 ml). The combined organic extracts were dried (MgSO4) and purified by preparative TLC hexanes:EtOAc (1:1) to give the subtitle compound (24.2 mg, 17%). MS calculated for C14H18BrNO2S+H 344, observed 344, 346.

WORKUP

后处理

  1. customNext, the reaction mixture was carefully quenched with sat. NaHCO3 (5 ml)
  2. extractionextracted with EtOAc (3×20 ml)
  3. dry with materialThe combined organic extracts were dried (MgSO4)
  4. custompurified by preparative TLC hexanes:EtOAc (1:1)