HRID2046992

反应详情

EQUATION

反应方程式

HRID 2046992 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

503 mg 2,4-dichloro-5-methyl-7H-pyrrolo[2,3-d]pyrimidine (5) (2.5 mmol) and 523 mg TsCl (2.75 mmol) were dissolved in 20 mL of DMF. After cooling to 0° C., 200 mg NaH (2.75 mmol) was slowly added under N2. The reaction mixture was stirred at 0° C. for 30 minutes and quenched by adding 10 mL of 10% aqueous NH4Cl at this temperature, then extracted with EtOAc (3×50 mL). Combined organic layers were washed with brine, dried over Na2SO4 and purified by flash column chromatography to give the title compound as light yellow solid.

WORKUP

后处理

  1. customquenched
  2. additionby adding 10 mL of 10% aqueous NH4Cl at this temperature
  3. extractionextracted with EtOAc (3×50 mL)
  4. washCombined organic layers were washed with brine
  5. dry with materialdried over Na2SO4
  6. custompurified by flash column chromatography