HRID2426107

反应详情

EQUATION

反应方程式

HRID 2426107 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-bromomethyl-4-chloro-1-methyl-1H-pyrazolo[3,4-d]pyrimidine (90.2 mg, 0.28 mmol, Example 5), 3-benzyloxy-phenol (75.2 mg, 0.36 mmol, TCl) and potassium carbonate (59.6 mg, 0.43 mmol) in dimethylformamide was stirred at room temperature overnight. The resulting mixture was concentrated under reduced pressure and the residue was dissolved in ethyl acetate, washed with water and brine, and dried and concentrated. The crude product was either used directly in the next step (described in Example 7) or purified by flash chromatography (silica gel, hexanes-ethyl acetate, 90/10 to 60/40) to give pure 3-(3-benzyloxy-phenoxymethyl)-4-chloro-1-methyl-1H-pyrazolo[3,4-d]pyrimidine. (Yield 33 mg).

WORKUP

后处理

  1. concentrationThe resulting mixture was concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with water and brine
  4. customdried
  5. concentrationconcentrated
  6. custompurified by flash chromatography (silica gel, hexanes-ethyl acetate, 90/10 to 60/40)