HRID6071

反应详情

EQUATION

反应方程式

HRID 6071 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred, 0° C. solution of 4-hydroxybenzonitrile (50.7 g, 426 mmol) in 1400 mL of dichloromethane and 75 mL anhydrous ethanol is treated with anhydrous hydrogen chloride gas (110 g) over 1.5 hours. This solution is stirred at room temperature for 64 hours and the resulting solids collected and washed with 500 mL diethyl ether and 2×1000 mL of ethyl acetate. The remaining solids (60.4 g) were dissolved in 1200 mL of water and the residual solids filtered. To the filtrate is added a solution of sodium hydroxide (12.57 g) in 150 mL water. The resulting white solid is filtered and washed with water to afford ethyl 4-hydroxybenzenecarboximidoate.

WORKUP

后处理

  1. customthe resulting solids collected
  2. washwashed with 500 mL diethyl ether and 2×1000 mL of ethyl acetate
  3. dissolutionThe remaining solids (60.4 g) were dissolved in 1200 mL of water
  4. filtrationthe residual solids filtered
  5. additionTo the filtrate is added a solution of sodium hydroxide (12.57 g) in 150 mL water
  6. filtrationThe resulting white solid is filtered
  7. washwashed with water