反应详情

To a stirring solution of Methyl 3-hydroxy-5-[4-(5-methyl-1,3,4-oxadiazol-2-yl)phenoxy]benzoate (4 g) (Intermediate 7) in dry DMF, 3-Bromo-1-methyl-pyrrolidine-2-one (4.12 g) (Intermediate 5) [J. Med. Chem., 1987, 30, 1995-98] was added under nitrogen atmosphere at room temperature in three portions at 4 h interval. The reaction mixture was stirred at room temperature for 16 h and then warmed to 45-50° C. for 3 h. The reaction was monitored by TLC. After completion, reaction mixture was diluted with ice cold water and extracted with EtOAc. All organic layers were combined and washed with water, brine, dried over anhydrous sodium sulphate, filtered and concentrated under vacuum to get crude thick liquid product. Crude residue was chromatographed to yield pure compound (5.2 g).

1. temperaturewarmed to 45-50° C. for 3 h
2. customAfter completion, reaction mixture
3. additionwas diluted with ice cold water
4. extractionextracted with EtOAc
5. washwashed with water, brine
6. dry with materialdried over anhydrous sodium sulphate
7. filtrationfiltered
8. concentrationconcentrated under vacuum
9. customto get crude thick liquid product
10. customCrude residue was chromatographed