HRID2197475

反应详情

EQUATION

反应方程式

HRID 2197475 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
170 °C

PROCEDURE

实验过程

2-chloroadenine (1) (1.60 g, 9.44 mmol) was divided among three microwave vials (10-20 mL), each containing Butylamine (4 mL), 1-Butanol (10 mL,), and DMSO (1 mL). Each vial was heated to 170° C. for 90 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 1.62 g (83%) of 64 as an off white solid. 1H NMR (300 MHz, DMSO) δ 0.877 (t, 3H), 1.29 (m, 2H), 1.45 (m, 2H), 3.17 (t, 2H), 6.49 (s, 2H), 7.61 (s, 1H), 12.1 (s, 1H). LCMS: m/z for C9H14N6++H observed 207.2 at 1.40 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