HRID17129

反应详情

EQUATION

反应方程式

HRID 17129 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of bromine (0.4 mL, 4.6 mmol) in dichloromethane (5 mL) was added dropwise to a −5° C. solution of Example 76A (1.57 g, 4.6 mmol) in dichloromethane (30 mL). The mixture was stirred at −5° C. to 0° C. for 15 minutes and quenched with 1:1 saturated NaHCO3 and saturated NaHSO3 (10 mL). The organic phase was separated, washed with water and brine, dried (Na2SO4), filtered, and concentrated to provide 1.85 g of the desired product. MS (ESI(+)) m/e 421 (M+H)+.

WORKUP

后处理

  1. customquenched with 1:1 saturated NaHCO3 and saturated NaHSO3 (10 mL)
  2. customThe organic phase was separated
  3. washwashed with water and brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated