HRID2189314

反应详情

EQUATION

反应方程式

HRID 2189314 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-chloro-7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidine-6-carbaldehyde (283 mg, 1.11 mmol) in DMF (3 mL) is added oxone (820 mg, 1.33 mmol) at room temperature. The mixture is stirred at room temperature for 5 h and is quenched with 20% Na2S2O3 aqueous solution. After stirring for 10 min, the reaction mixture is acidified with 1N HCl aqueous solution (pH=5). The mixture is extracted with dichloromethane, dried over Na2SO4 and concentrated in vacuo. The solid is filtered, washed with acetonitrile, and dried under vacuum to give 130 mg of 2-chloro-7-(1-ethyl-propyl)-7H-pyrrolo[2,3-d]pyrimidine-6-carboxylic acid as a pale brown solid.

WORKUP

后处理

  1. customis quenched with 20% Na2S2O3 aqueous solution
  2. stirringAfter stirring for 10 min
  3. extractionThe mixture is extracted with dichloromethane
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated in vacuo
  6. filtrationThe solid is filtered
  7. washwashed with acetonitrile
  8. customdried under vacuum