HRID964622

反应详情

EQUATION

反应方程式

HRID 964622 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of (R)-2-bromo-1-[4-phenylmethoxy-3-[(methylsulfonyl)amino]phenyl]ethanol (12.4 g, 31 mmol) and NaI (52 g, 346 mmol) were refluxed in acetone (190 mL) for 1.75 hours. After filtration, the filtrate was concentrated to a pasty red-brown solid which was partitioned between CH2Cl2 (150 mL) and H2O (190 mL). The organic phase was washed with 150 mL ~23.5% w/w aq. sodium bisulfite and with H2O (150 mL), dried over Na2SO4 and concentrated to give the title compound (12.72 g, 91%).

WORKUP

后处理

  1. filtrationAfter filtration
  2. concentrationthe filtrate was concentrated to a pasty red-brown solid which
  3. customwas partitioned between CH2Cl2 (150 mL) and H2O (190 mL)
  4. washThe organic phase was washed with 150 mL ~23.5% w/w aq. sodium bisulfite and with H2O (150 mL)
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated