HRID2197472

反应详情

EQUATION

反应方程式

HRID 2197472 的结构方程式

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

2-chloroadenine (1) (1.53 g, 9.03 mmol) was divided among three microwave vials (10-20 mL), each containing 1-butanol (10 mL) and t-BuOK (5 mL, 1M in THF). Each vial was heated to 170° C. for 40 minutes. After reaction completion the solvent was removed by rotary evaporation and the product was purified on flash column eluting 10% methanol in ethylacetate. Evaporation of solvent gave 1.33 g (70%) of 59 as an off white solid. 1H NMR (300 MHz, DMSO) δ 0.919 (t, 3H), 1.39 (m, 2H), 1.62 (m, 2H), 4.09 (t, 2H), 6.00 (s, 2H), 7.44 (s, 1H). LCMS: m/z for C9H13N5O++H observed 208.1 at 1.34 minutes of a 3.5 minute run, gradient 5-95% CH3CN in H2O.

WORKUP

后处理

  1. customAfter reaction completion the solvent
  2. customwas removed by rotary evaporation
  3. customthe product was purified on flash column
  4. washeluting 10% methanol in ethylacetate
  5. customEvaporation of solvent