HRID529645

反应详情

EQUATION

反应方程式

HRID 529645 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

A solution of 6-(2,4-dichloro-7-((2-(trimethylsilyl)ethoxy)methyl)-7H-pyrrolo[2,3-d]pyrimidin-5-yl)-2-methylbenzo[d]oxazole (1 equiv), cyclopentanol (1.1 equiv), and sodium tert-butoxide (1 equiv) in 1,4-dioxane (0.22 M) was taken in a sealable flask. The reaction mixture was put under a nitrogen atmosphere, the sealable flask was sealed and the mixture was stirred at 70° C. for 3 h. The mixture was cooled to room temperature and concentrated to afford an oil, which was suspended in DCM and loaded onto a silica column (packed with hexanes). The column was eluted with 0-30% ethyl acetate in hexanes. The fractions containing product were combined and concentrated to dryness to give the target product as a light yellow oil (Yield: 88%) that solidified upon standing. MS (ESI) m/z 499.4 [M+1]+.

WORKUP

后处理

  1. customthe sealable flask was sealed
  2. temperatureThe mixture was cooled to room temperature
  3. concentrationconcentrated
  4. customto afford an oil, which
  5. washThe column was eluted with 0-30% ethyl acetate in hexanes
  6. additionThe fractions containing product
  7. concentrationconcentrated to dryness