HRID542247
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureis heated
- customThe residue in the amount of 2.6 g is separated
- additionadded with 15 ml of glacial acetic acid, 8 ml of distilled water, 1.8 g of sodium nitrite
- customThe solution is evaporated
- customthe residue is recrystallized from methanol
- customto give 2.32 g (80% of the theoretical) of the product