HRID384745

反应详情

EQUATION

反应方程式

HRID 384745 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
35 °C

PROCEDURE

实验过程

5-(2-Amino-[1,2,4]triazolo[1,5-a]pyridin-6-yl)-pyridine-3-sulfonic acid tert-butylamide (50 mg, 0.14 mmol) was suspended in tetrahydrofuran:pyridine (30 mL, 5:1) and cooled to 0° C. Triphosgene (41 mg, 0.14 mmol) was added in one portion and the reaction mixture heated at 35° C. for 2 hours. After this time the solvent was decanted and the resultant semi-solid dissolved in DMF:pyridine (1 mL, 10:1), N-Boc-ethylenediamine (50 mg, 0.32 mmol) was added in one portion and the reaction mixture heated for 18 hours at 65° C. The desired product was isolated as a white solid, directly from the reaction mixture, by preparative HPLC (35 mg)

WORKUP

后处理

  1. customAfter this time the solvent was decanted
  2. dissolutionthe resultant semi-solid dissolved in DMF
  3. temperaturethe reaction mixture heated for 18 hours at 65° C