HRID1452623
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 40 °C
PROCEDURE
实验过程
To an isopropanol (3 mL) solution containing 3-(5,7-dichloropyrazolo[1,5-a]pyrimidin-6-yl)propan-1-ol (224 mg, 0.910 mmol), triethylamine (253 μL, 1.82 mmol) and phenethidine (128 μL, 1.00 mmol) were added, and this mixture was stirred at 40° C. for 5 hr. After the reaction, the solvent was distilled off, aqueous sodium hydrogen carbonate was added to the residue, and the mixture was extracted with ethyl acetate. The combined ethyl acetate layer was dried over sodium sulfate. After the sodium sulfate was filtered off, the filtrate was concentrated and the residue was purified with column chromatography (30% ethyl acetate-hexane) to obtain the title compound (212 mg).
WORKUP
后处理
- additionwere added
- customAfter the reaction
- distillationthe solvent was distilled off
- additionaqueous sodium hydrogen carbonate was added to the residue
- extractionthe mixture was extracted with ethyl acetate
- dry with materialThe combined ethyl acetate layer was dried over sodium sulfate
- filtrationAfter the sodium sulfate was filtered off
- concentrationthe filtrate was concentrated
- customthe residue was purified with column chromatography (30% ethyl acetate-hexane)