HRID542248

反应详情

EQUATION

反应方程式

HRID 542248 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-1 °C

PROCEDURE

实验过程

A mixture of 3.6 g of D-glucose, 2.8 g of butylurea, 0.2 g of nitroaniline and 0.15 ml of a concentrated hydrochloric acid in 10 ml of methanol is heated at reflux for 20 minutes. The resulting precipitate in the amount of 3 g is separated and added with 15 ml of glacial acetic acid, 10 ml of distilled water, 1.8 g of sodium nitrite and stirred at the temperature of -1° C. for 2 hours to give 2.98 g of the product (90% of the thoretical), hydroscopic, [α]D -1° (CH3OH), Rf =0.85. Found, %: N 13.47. Calculated, % N 13.68.

WORKUP

后处理

  1. temperatureis heated
  2. temperatureat reflux for 20 minutes
  3. customThe resulting precipitate in the amount of 3 g is separated
  4. additionadded with 15 ml of glacial acetic acid, 10 ml of distilled water, 1.8 g of sodium nitrite