反应详情

Sodium hydride suspension (0.16 g, 50%) was added to a stirring solution of (R)-(+)-Methyl 3-(4-(5-methyl-1,3,4-oxadiazol-2-yl)phenoxy)-5-((2-oxopyrrolidin-3-yl)oxy)benzoate (1.5 g) (Intermediate 20) in dry DMF taken in a round bottomed flask fitted with anhydrous CaCl2 guard tube, at room temperature. The reaction mixture was stirred at the same temperature for 15 min. Methyl iodide (0.20 mL) was added and stirred till the reaction completed. The reaction mixture was quenched with ice-water, extracted with DCM. All organic layers were combined, washed with water, brine, dried over sodium sulphate, filtered and concentrated in vacuum to get the thick liquid product. The liquid was triturated with EtOAc:hexane to get the white solid product (1.2 g).

1. customtaken in a round bottomed flask
2. customfitted with anhydrous CaCl2 guard tube, at room temperature
3. stirringstirred till the reaction
4. customThe reaction mixture was quenched with ice-water
5. extractionextracted with DCM
6. washwashed with water, brine
7. dry with materialdried over sodium sulphate
8. filtrationfiltered
9. concentrationconcentrated in vacuum
10. customto get the thick liquid product
11. customThe liquid was triturated with EtOAc