HRID645702

反应详情

EQUATION

反应方程式

HRID 645702 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2,4-dichloro-5-iodo-7H-pyrrolo[2,3-d]pyrimidine (1.80 g, 5.73 mmol) in CH2Cl2 (20 mL) was added p-toluenesulfonyl chloride (TsCl) (1.09 g, 5.73 mmol) and triethylamine (TEA) (1.60 mL, 11.46 mmol), followed by dimethylaminopyridine (DMAP) (70 mg, 0.573 mmol). After stirring for 1 h at room temperature, the solution was concentrated, and the residue was partitioned between ethyl acetate and H2O. The organic layer was separated, washed sequentially with 1N HCl and 5% NaHCO3. The organic extracts were dried over Na2SO4 and concentrated to give 2,4-dichloro-5-iodo-7-tosyl-7H-pyrrolo[2,3-d]pyrimidine (2.0 g).

WORKUP

后处理

  1. concentrationthe solution was concentrated
  2. customthe residue was partitioned between ethyl acetate and H2O
  3. customThe organic layer was separated
  4. washwashed sequentially with 1N HCl and 5% NaHCO3
  5. dry with materialThe organic extracts were dried over Na2SO4
  6. concentrationconcentrated