HRID589981

反应详情

EQUATION

反应方程式

HRID 589981 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

4-(4-Sulfamoyl-4,7-diaza-spiro[2.5]oct-7-yl)-pyrrolo[2,3-d]pyrimidine-7-carboxylic acid tert-butyl ester (intermediate 2) (0.049 mmol) was dissolved in dry DMF (1 mL) and added Cs2CO3 (0.147 mmol) and 2-bromopentane (0.074 mmol). Stirred at 60° C. for 16 h and then filtered through a syringe filter. The obtained filtrate was added 2,2,2-trifluoroethanol (1 mL) and heated to 100° C. for 1 h. The pure compound was obtained by standard preparative HPLC purification of the reaction mixture.

WORKUP

后处理

  1. filtrationfiltered through a syringe
  2. filtrationfilter
  3. additionThe obtained filtrate was added 2,2,2-trifluoroethanol (1 mL)
  4. temperatureheated to 100° C. for 1 h
  5. customThe pure compound was obtained by standard preparative HPLC purification of the reaction mixture