反应详情

To a solution of 5-(5-(3-chloropropylthio)-4-methyl-4H-1,2,4-triazol-3-yl)-2,4-dimethylthiazole (Prep28, 70 mg, 0.23 mmol) in dry NMP (1 ml), K2CO3 (0.144 g, 1 mmol) was added and stirred for 10 min, then 5-chloro-2,3-dihydrospiro[indene-1,3′-pyrrolidine]hydrochloride (Prep10, 88 mg, 0.36 mmol) and NaI (0.07 g) were added and stirred for 23 h at 65° C. Water was then added and the solution was extracted with ethyl acetate (2×10 ml). The organic phase was washed with brine, dried over Na2SO4 and concentrated in vacuo. The crude product was purified by P-HPLC (TLC analysis performed by eluting with EA/MeOH 80:10) to give 57 mg of the title compound (y=52%).

1. stirringstirred for 23 h at 65° C
2. extractionthe solution was extracted with ethyl acetate (2×10 ml)
3. washThe organic phase was washed with brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated in vacuo
6. customThe crude product was purified by P-HPLC (TLC analysis performed by eluting with EA/MeOH 80:10)