反应详情

A solution of 2-(3-hydroxypropyl)benzonitrile (Example 323c, 3.83 g) in DMF (40 mL) under nitrogen was treated with 60% Sodium hydride (1.140 g) and stirred at room temperature for 1 h before adding benzyl bromide (2.83 mL). The resulting solution was stirred at 20° C. for 60 h. The reaction mixture was diluted with water (200 mL), and extracted with ethyl acetate (200 mL). The organic was dried (MgSO4), filtered and evaporated. The residue was purified (SiO2 chromatography eluting with 30% diethyl ether in isohexane). Pure fractions were evaporated to dryness to afford the subtitle compound as an oil (2.3 g).

1. stirringThe resulting solution was stirred at 20° C. for 60 h
2. extractionextracted with ethyl acetate (200 mL)
3. dry with materialThe organic was dried (MgSO4)
4. filtrationfiltered
5. customevaporated
6. customThe residue was purified
7. wash(SiO2 chromatography eluting with 30% diethyl ether in isohexane)
8. customPure fractions were evaporated to dryness