HRID1487245

反应详情

EQUATION

反应方程式

HRID 1487245 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

5-((Benzyloxy)methyl)-2-butyl-4-chloro-7-iodo-5H-pyrrolo[3,2-d]pyrimidine (1 g, 2.2 mmol) was suspended in 2-propanol (5 mL) and 35% (0.88) ammonia solution (4 mL). The reaction was stirred at 120° C. for 90 minutes in a Biotage Initiator microwave. A further 1 mL of 35% (0.88) ammonia solution was added to the reaction. The reaction was stirred at 120° C. for 90 minutes in a Biotage Initiator microwave. The reaction was evaporated in vacuo to yield a pale yellow oil. The oil was dissolved in the minimum volume of 20% methanol in dichloromethane and purified by chromatography on silica using a gradient of 0-100% ethyl acetate in cyclohexane gradient over 80 minutes. Fractions were combined and evaporated in vacuo to yield the title compound as a colourless oil (768 mg).

WORKUP

后处理

  1. stirringThe reaction was stirred at 120° C. for 90 minutes in a Biotage Initiator microwave
  2. customThe reaction was evaporated in vacuo
  3. customto yield a pale yellow oil
  4. custompurified by chromatography on silica using a gradient of 0-100% ethyl acetate in cyclohexane gradient over 80 minutes
  5. customevaporated in vacuo