HRID2047056

反应详情

EQUATION

反应方程式

HRID 2047056 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

7-chloro-5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrazolo[1,5-a]pyrimidine (5.58 mmol, 1.64 g) is charged to 10-20 mL microwave vessel. To this vessel is added 10 mL ˜7N NH3 in methanol. The vessel was sealed and heated at 100° C. for 18 hours. After 18 hours, the reaction mixture was cooled to room temperature and diluted with 100 mL DCM. The resulting solution is washed with saturated NaHCO3(aq) and extracted with DCM twice more. The combined organics were dried over Na2SO4 and the solvent removed in vacuo to yield 5-(1,4-dioxaspiro[4.5]decan-8-yl)pyrazolo[1,5-a]pyrimidin-7-amine (1.52 g, 99% yield) as pale orange solid.

WORKUP

后处理

  1. customThe vessel was sealed
  2. temperaturethe reaction mixture was cooled to room temperature
  3. washThe resulting solution is washed with saturated NaHCO3(aq)
  4. extractionextracted with DCM twice more
  5. dry with materialThe combined organics were dried over Na2SO4
  6. customthe solvent removed in vacuo