HRID542246

反应详情

EQUATION

反应方程式

HRID 542246 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 3 g of D-xylose, 1.9 g of ethylurea, 0.3 g of nitroaniline and 0.2 ml of a concentrated hydrochloric acid is refluxed in 15 ml of ethanol for 10 minutes. The precipitate in the amount of 2.8 g is separated, then added with 15 ml of glacial acetic acid, 2.5 ml of distilled water and 1.74 g of sodium nitrite and stirred for 2 hours at 0° C. The solution is evaporated and recrystallized from an alcohol to give 2.54 g (80% of the theoretical) of the product. M.p. 104° C. (decomposition), [α]D -13.6° (water), Rf =0.76. Found, %: N 16,42. Calculated, %: N 16.86.

WORKUP

后处理

  1. customThe precipitate in the amount of 2.8 g is separated
  2. additionadded with 15 ml of glacial acetic acid, 2.5 ml of distilled water and 1.74 g of sodium nitrite
  3. customThe solution is evaporated
  4. customrecrystallized from an alcohol
  5. customto give 2.54 g (80% of the theoretical) of the product