HRID902099

反应详情

EQUATION

反应方程式

HRID 902099 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
135 °C

PROCEDURE

实验过程

A solution of 10.0 grams (0.085 mole) of para-toluonitrile in 160 mL of DMF was stirred and 5.6 grams (0.085 mole) of sodium azide was added. Upon completion of addition, the reaction mixture was warmed to 135° C. where it stirred for three hours. The reaction mixture was then cooled and poured into 200 mL of stirred, cold aqueous 1N hydrochloric acid. Upon completion of addition, the mixture was stirred for five minutes and filtered to collect a white solid. The solid was dried for 16 hours in a vacuum oven at 35-40° C., yielding 7.1 grams of the subject compound. The reaction was repeated.

WORKUP

后处理

  1. additionUpon completion of addition
  2. temperatureThe reaction mixture was then cooled
  3. additionpoured into 200 mL
  4. stirringof stirred
  5. additionUpon completion of addition
  6. stirringthe mixture was stirred for five minutes
  7. filtrationfiltered
  8. customto collect a white solid
  9. customThe solid was dried for 16 hours in a vacuum oven at 35-40° C.