HRID904771

反应详情

EQUATION

反应方程式

HRID 904771 的结构方程式

PROCEDURE

实验过程

A solution of 9.0 g of the product of Example 3, 4.2 g of butyl isocyanate and 0.1 g of DABCO in 80 ml of dry xylenes was heated to 136°. To this solution was added 3.0 ml of liquid phosgene at such a rate as to maintain the temperature between 125° and 136°. This addition required about 21/2 hours. The solution was cooled to 25°, filtered under nitrogen and stripped in vacuo to give crude 2-nitrophenylmethanesulfonyl isocyanate as a viscous, moisture-sensitive oil showing a sulfonyl isocyanate peak in the infrared at 2230 cm-1.

WORKUP

后处理

  1. temperatureto maintain the temperature between 125° and 136°
  2. additionThis addition
  3. custom2 hours
  4. temperatureThe solution was cooled to 25°
  5. filtrationfiltered under nitrogen