HRID77461

反应详情

EQUATION

反应方程式

HRID 77461 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To the solution of 2-aminopyrimidin-5-ol (0.500 g, 4.50 mmol) in dry MeOH (10 mL), K2CO3 (0.622 g, 4.50 mmol) and benzyl bromide (0.535 mL, 4.50 mmol) were added. The reaction mixture was stirred at room temperature for 18 h. Solvent was removed under reduced pressure. The residue was dissolved in ethyl acetate and washed with water and brine, then dried over sodium sulfate. The crude product was purified by flash chromatography on silica gel using 50% ethyl acetate in petroleum ether. The desired fractions were concentrated to give 5-(benzyloxy)pyrimidin-2-amine as an off-white solid (0.222 g 25%). 1HNMR 400 MHz, DMSO-d6: δ ppm 5.06 (s, 2H), 6.21 (s, 2H), 7.28-7.30 (m, 5H), 7.45 (s, 2H). LCMS: RT 1.060 min; 202.2 (M+H).

WORKUP

后处理

  1. customSolvent was removed under reduced pressure
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washwashed with water and brine
  4. dry with materialdried over sodium sulfate
  5. customThe crude product was purified by flash chromatography on silica gel using 50% ethyl acetate in petroleum ether
  6. concentrationThe desired fractions were concentrated