HRID1817899

反应详情

EQUATION

反应方程式

HRID 1817899 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-bromo-N1-[2-(trifluoromethoxy)ethyl]benzene-1,2-diamine (step B, 752 mg, 2.51 mmol) in ethyl acetate (22 mL) was added tert-butylacetyl chloride (355 mg, 2.64 mmol) at room temperature. After stirring for 2 h at room temperature, the mixture was diluted with ethyl acetate. The organic solution was washed with saturated sodium hydrogencarbonate aqueous solution, brine, dried over magnesium sulfate and concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=4:1 as eluent) to afford the title compound (728 mg, 73%) as a white solid.

WORKUP

后处理

  1. washThe organic solution was washed with saturated sodium hydrogencarbonate aqueous solution, brine
  2. dry with materialdried over magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by column chromatography on silica gel (hexane:ethyl acetate=4:1 as eluent)