HRID705369

反应详情

EQUATION

反应方程式

HRID 705369 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A solution of 4-chloro-3-methoxyaniline (1.0 equivalent) dissolved in CH2Cl2 (15 volumes) at 5° C. was treated portion wise with N-bromosuccinimide (1.03 equivalents), warmed to 20° C. and mixed for 5 minutes. A 5% aqueous Na2SO3 solution (10 volumes) was added and the mixture was stirred for 10 minutes. The layers were separated and the organic layer was washed with water and saturated brine, dried (Na2SO4), filtered and concentrated. The resulting solid was triturated with a minimal volume of heptane and the solid was collected by filtration and dried to constant mass (80% yield).

WORKUP

后处理

  1. additionmixed for 5 minutes
  2. customThe layers were separated
  3. washthe organic layer was washed with water and saturated brine
  4. dry with materialdried (Na2SO4)
  5. filtrationfiltered
  6. concentrationconcentrated
  7. customThe resulting solid was triturated with a minimal volume of heptane
  8. filtrationthe solid was collected by filtration
  9. customdried to constant mass (80% yield)