HRID486749

反应详情

EQUATION

反应方程式

HRID 486749 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 4.05 g (24.8 mmole) of N-Pentylaniline (from Step A) in 45 ml of toluene an 8.96 ml (24.8 mmole) of 2.77N NaOH were mechanically stirred at -5° C., and 25.7 ml (49.6 mmole) of 1.93M phosgene in toluene was added dropwise over 30 minutes while maintaining -5°. After half the phosgene solution had been added, the rate of addition was increased easily. After stirring at -5° for an additional 30 minutes, the phases were separated and the toluene layer was dried over 10 g of solid sodium chloride. Concentration gave 5.5 g (98%) of dark yellow oil.

WORKUP

后处理

  1. temperaturewhile maintaining -5°
  2. additionthe rate of addition
  3. temperaturewas increased easily
  4. customthe phases were separated
  5. dry with materialthe toluene layer was dried over 10 g of solid sodium chloride
  6. concentrationConcentration