HRID1678772

反应详情

EQUATION

反应方程式

HRID 1678772 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a stirred solution of 11-3 (0.2 g, 0.36 mMol), HOBT (0.05 g, 0.4 mMol), and 1H-1,2,3-triazole-4-carboxylic acid (0.05 g, 0.4 mMol) in anhydrous DMF (2 mL) was added DIEA (0.18 mL, 1.1 mMol) followed by EDC (0.08 g, 0.4 mMol). The solution was heated in the microwave reactor for 30 minutes at 80° C. Solution was then treated with 0.5 mL of acetic acid and was heated to 80° C. in the microwave reactor for 10 min. Upon cooling to room temperature, the solution was passed through a syringe filter and purified on a C18 reverse phase HPLC to give 11-4 as a solid. Mass (M+1) calculated: 632.2742 observed: 632.274

WORKUP

后处理

  1. temperaturewas heated to 80° C. in the microwave reactor for 10 min
  2. temperatureUpon cooling to room temperature
  3. customthe solution was passed through a syringe
  4. filtrationfilter
  5. custompurified on a C18 reverse phase HPLC