HRID1884350

反应详情

EQUATION

反应方程式

HRID 1884350 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 3-[2,5,6-trimethyl-7-(2,4,6-trimethyl-phenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-yl]-pentan-3-ol (0.041 g, 0.122 mmol), concentrated sulfuric acid (0.055 g, 0.56 mmol) and acetic acid (0.136 g, 2.27 mmol) was heated to reflux for 1 hour, cooled, diluted with water, basified to pH10 with 2 N NaOH and extracted with ethyl acetate. The organic layer was washed with brine, dried and concentrated to dryness to give 43 mg of the title compound as a clear oil. The oil was purified through silica gel column chromatography to give 40 mg of the title compound as a white solid, mp 59-61° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 1 hour
  3. temperaturecooled
  4. extractionextracted with ethyl acetate
  5. washThe organic layer was washed with brine
  6. customdried
  7. concentrationconcentrated to dryness