反应详情

To a stirring solution of S-(+3-[4-(5-Methyl-1,3,4-oxadiazol-2-yl)phenoxy]-5-[(1-methyl-2-oxo-pyrrolidin-3-yl)oxy]benzoic acid (3.5 g) (Intermediate 13) in dry DCM in single necked round bottomed flask fitted with stop cock with N2(g) balloon, 4-(dimethylamino)pyridine (2.24 g) followed by N-(3-Dimethylaminopropyl)-N′-ethylcarbodiimide hydrochloride (EDCI. HCl) (3.3 g) were added at room temperature. After stirring at the same temperature for 15 min, 2-aminothiazole (0.94 g) was added and stirring was continued for 16 h. Progress of reaction was monitored by TLC. After completion, reaction mixture was diluted with DCM (200 mL), washed with dil HCl (20 mL, 0.05 N), saturated sodium bicarbonate solution, water and brine, dried over anhydrous sodium sulphate, filtered and concentrated under vacuum to get crude brown solid (3.5 g). The crude brown solid was purified by solvent trituration.

1. additionwere added at room temperature
2. stirringstirring
3. waitwas continued for 16 h
4. customProgress of reaction
5. customAfter completion, reaction mixture
6. washwashed with dil HCl (20 mL, 0.05 N), saturated sodium bicarbonate solution, water and brine
7. dry with materialdried over anhydrous sodium sulphate
8. filtrationfiltered
9. concentrationconcentrated under vacuum