HRID45000

反应详情

EQUATION

反应方程式

HRID 45000 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Morpholine (0.19 mL, 0.0022 mol) in 1.0 ml of THF was added dropwise to a solution of 3-bromobenzenesulfonyl chloride (0.3 mL, 0.002 mol) and TEA (0.30 mL, 0.0022 mol) in dry 4.0 mL of THF cooled in an ice bath. The reaction mixture was stirred overnight at room temperature and was then partitioned between 0.05N HCl and ethyl acetate. The organic layer was washed with water (2×), and brine (1×), and was then dried over anhydrous magnesium sulfate, filtered and then was concentrated in vacuo to give 4-[(3-bromophenyl)sulfonyl]morpholine as a white crystalline product (470 mg, 78%). LCMS (M+H)+: m/z=306, 308.

WORKUP

后处理

  1. temperaturecooled in an ice bath
  2. customwas then partitioned between 0.05N HCl and ethyl acetate
  3. washThe organic layer was washed with water (2×), and brine (1×)
  4. dry with materialwas then dried over anhydrous magnesium sulfate
  5. filtrationfiltered
  6. concentrationwas concentrated in vacuo