HRID2093923

反应详情

EQUATION

反应方程式

HRID 2093923 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(5-Cyclopropylmethoxy-1,3-benzodioxol-4-yl)-5H-pyrrolo[3,2-d]pyrimidine-7-carboxylic acid piperidin-4-ylamide hydrochloride from example A138 (472 mg; 1.0 mmol) and DBU (2.5 mmol) is dissolved in dry dichloromethane (5 mL). Propionyl chloride (1.1 mmol) is syringed into the reaction mixture at ice bath temperature. After complete addition stirring is continued at ambient temperature over night. Methanol (1 mL) is added and stirring is continued for two hours. The volatiles are evaporated. The residue is purified by reversed phase preparative HPLC. The collected product fraction is freeze-dried to yield 375 mg of the title compound as colorless solid.

WORKUP

后处理

  1. additionAfter complete addition
  2. waitis continued at ambient temperature over night
  3. stirringstirring
  4. customThe volatiles are evaporated
  5. customThe residue is purified by reversed phase preparative HPLC
  6. customThe collected product fraction is freeze-dried