反应详情

Sodium hydride suspension (0.71 g, 50%) was added to a stirring solution of (S)-(−)-methyl 3-(4-(5-methyl-1,3,4-oxadiazol-2-yl)phenoxy)-5-((2-oxopyrrolidin-3-yl)oxy)benzoate (5.5 g) (Intermediate 15) 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 (0.91 mL) was added and stirred till the reaction completion. 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 vaccuo to get the thick liquid product. The liquid was triturated with EtOAc:hexane to get the white solid product (5.3 g).

1. customtaken in a round bottomed flask
2. customfitted with anhydrous CaCl2 guard tube at room temperature
3. stirringstirred till the reaction completion
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 vaccuo
10. customto get the thick liquid product
11. customThe liquid was triturated with EtOAc