HRID1014931

反应详情

EQUATION

反应方程式

HRID 1014931 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of the product from Example 4A (4.2 g, est. 18 mmol), guanidine chloride (7.1 g, 72.8 mmol), and K2CO3 (10.8 g, 78 mmol) in DMF (30 mL) was heated to 125° C. for 3 hours. The mixture was cooled and the solids were removed by filtration. The solids were washed with EtOAc. The combined filtrates were concentrated under reduced pressure and the residue was passed through silica gel pad eluting with EtOAc:hexanes (8:2) and then with MeOH:EtOAc:CH2Cl2 (10:45:45) to provide the title compound as a white solid (2.8 g).

WORKUP

后处理

  1. temperatureThe mixture was cooled
  2. customthe solids were removed by filtration
  3. washThe solids were washed with EtOAc
  4. concentrationThe combined filtrates were concentrated under reduced pressure
  5. washeluting with EtOAc:hexanes (8:2)