HRID4112

反应详情

EQUATION

反应方程式

HRID 4112 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 7.7 g (25 mmol) of 3,4-dibenzyloxyaniline in 50 ml of 1:1 acetonitrile/water at 0° C. was added chloroacetyl chloride (3.0 ml) while keeping the pH at 6.5 with saturated aqueous potassium bicarbonate. When the pH remained constant for 15 minutes, an additional 3 ml of chloroacetyl chloride was added in small portions while maintaining the pH at 6.5. When the pH remained constant for 15 minutes, the acetonitrile was evaporated, and the resulting aqueous solution was filtered. The precipitate was washed thoroughly with water to yield, upon drying in vacuo, 8.98 g of the title compound.

WORKUP

后处理

  1. temperaturewhile maintaining the pH at 6.5
  2. waitWhen the pH remained constant for 15 minutes
  3. customthe acetonitrile was evaporated
  4. filtrationthe resulting aqueous solution was filtered
  5. washThe precipitate was washed thoroughly with water
  6. customto yield
  7. dry with materialupon drying in vacuo, 8.98 g of the title compound