HRID542247

反应详情

EQUATION

反应方程式

HRID 542247 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, 2.3 g of propylurea, 0.2 g of nitroaniline and 0.1 ml of a concentrated sulphuric acid is heated at reflux for 10 minutes in 15 ml of methanol. The residue in the amount of 2.6 g is separated, added with 15 ml of glacial acetic acid, 8 ml of distilled water, 1.8 g of sodium nitrite and stirred at the temperature of -1° C. for 2 hours. The solution is evaporated, the residue is recrystallized from methanol to give 2.32 g (80% of the theoretical) of the product. M.p. 110° C. (decomposition), [α]D -5° (CH3OH), Rf =0.81. Found, %: N 14.12. Calculated, %: N 14.33.

WORKUP

后处理

  1. temperatureis heated
  2. customThe residue in the amount of 2.6 g is separated
  3. additionadded with 15 ml of glacial acetic acid, 8 ml of distilled water, 1.8 g of sodium nitrite
  4. customThe solution is evaporated
  5. customthe residue is recrystallized from methanol
  6. customto give 2.32 g (80% of the theoretical) of the product