HRID881798
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 170 °C
PROCEDURE
实验过程
2-chloroadenine (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. The three reaction mixtures were combined, 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 2-butoxy-9H-purin-6-amine (6) as an off white solid. 1H NMR (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
- customThe three reaction mixtures
- customthe solvent was removed by rotary evaporation
- customthe product was purified on flash column
- washeluting 10% methanol in ethylacetate
- customEvaporation of solvent