HRID1926871
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
- 160 °C
PROCEDURE
实验过程
Heat 2.0 g (8.67 mmol) 4-chloro-6-phenylfuro[2,3-d]pyrimidine and 6.04 ml (34.7 mmol) DIEA in 5 ml DMF to 160° C. Add 3.15 g (17.34 mmol) 6-aminohexanoic acid methyl ester hydrochloride and stir for 4 h at 160° C. After cooling, add the mixture to ice water and extract three times with ethyl acetate. Combine the organic phases and wash with saturated ammonium chloride solution, dry over magnesium sulphate and concentrate under vacuum. Add methanol to the oil residue. Filter off the precipitated solid with suction, wash with methanol again and dry the solid at high vacuum. 1.85 g (57.2% of theor.) of the target compound is obtained.
WORKUP
后处理
- temperatureAfter cooling
- extractionextract three times with ethyl acetate
- washwash with saturated ammonium chloride solution
- dry with materialdry over magnesium sulphate
- concentrationconcentrate under vacuum
- filtrationFilter off the precipitated solid with suction
- washwash with methanol again
- customdry the solid at high vacuum
- custom1.85 g (57.2% of theor.) of the target compound is obtained