HRID1085535

反应详情

EQUATION

反应方程式

HRID 1085535 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

0.16 g of 5'-azido-2',5'-dideoxy-5-(2-chloroethyl)uridine was dissolved in 100 ml of methanol and 1.9 ml of a 0.27M solution of hydrogen chloride in methanol was added. A slurry of 25 mg of 5% palladium-on-charcoal catalyst in 10 ml of ethanol was added under a nitrogen atmosphere and the mixture was hydrogenated at room temperature and under atmospheric pressure for 2 hours. The catalyst was removed by filtration and the filtrate was evaporated to give a solid which, after crystallization from a mixture of 15 ml of methanol and 30 ml of diethyl ether, gave 0.13 g of 5'-amino-5-(2-chloroethyl)-2',5'-dideoxyuridine hydrochloride of melting point 229°-230° C. (decomposition).

WORKUP

后处理

  1. customThe catalyst was removed by filtration
  2. customthe filtrate was evaporated
  3. customto give a solid which
  4. customafter crystallization
  5. additionfrom a mixture of 15 ml of methanol and 30 ml of diethyl ether