HRID1826539

反应详情

EQUATION

反应方程式

HRID 1826539 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To 1.50 g of 4-[6-amino-8-(3-fluorophenyl)-2-iodo-9H-9-purinyl]butanol were added 30 ml of chloroform, 30 ml of acetonitrile, 45 ml of water, 73 mg of ruthenium tetraoxide hydrate and4.10 g of sodium periodate and the mixture was vigorously stirred in a nitrogen stream for 5 hours at room temperature. The reaction was stopped by 2-propanol and the insoluble matters were filtered off followed by washing with 1000 ml of chloroform-methanol (1:1). The filtrate was concentrated, the residue was suspended in water, and the suspension was adjusted to pH 2-3 with 1N hydrochloric acid and the crystals were collected by filtration. The crystals were washed with water and ether to give 1.41 g of the title compound. The yield was 91%.

WORKUP

后处理

  1. filtrationthe insoluble matters were filtered off
  2. washby washing with 1000 ml of chloroform-methanol (1:1)
  3. concentrationThe filtrate was concentrated
  4. filtrationthe crystals were collected by filtration
  5. washThe crystals were washed with water and ether