HRID853285
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 140 °C
PROCEDURE
实验过程
After adding 200 ml of phosphorus oxychloride to 20 g of the 6-(4-benzyloxyphenyl)-7H-pyrrolo[2,3-d]pyrimidin-4-ol synthesized in Production Example 153-2, the mixture was stirred at 140° C. for 3 hours and the reaction mixture was cooled to room temperature and the reaction mixture was concentrated. Ice water was added to the residue, and liquid separation and extraction were performed with an ethyl acetate:tetrahydrofuran (5:1) mixed solvent. The organic layer was washed with water and saturated brine, dried over sodium sulfate and concentrated to dryness to obtain 12 g of the title compound.
WORKUP
后处理
- customsynthesized in Production Example 153-2
- temperaturethe reaction mixture was cooled to room temperature
- concentrationthe reaction mixture was concentrated
- additionIce water was added to the residue, and liquid separation and extraction
- additionmixed solvent
- washThe organic layer was washed with water and saturated brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated to dryness