反应详情

温度

70 °C

The mixture of 5-chloro-6-methoxy-2,3-dihydrospiro[indene-1,3′-pyrrolidine] (Prep19, 58 mg, 0.24 mmol), 5-(5-(3-chloropropylthio)-4-methyl-4H-1,2,4-triazol-3-yl)-2,4-dimethylthiazole (Prep28, 50 mg, 0.17 mmol), K2CO3 (68.5 mg, 0.50 mmol) and NaI (24.5 mg, 0.50 mmol) in NMP (1 ml) was warmed to 70° C., and stirred overnight. The mixture was extracted with EA (5 ml×2). The combined organic layers were washed with Sat. NaHCO3, brine and dried over Na2SO4. The organic layer was concentrated in vacuo to afford crude product. The crude was purified by P-TLC and P-HPLC and treated with a 1N solution of HCl in ether, then freeze-dried to afford title compound (10 mg, y=11.98%).

1. extractionThe mixture was extracted with EA (5 ml×2)
2. washThe combined organic layers were washed with Sat. NaHCO3, brine
3. dry with materialdried over Na2SO4
4. concentrationThe organic layer was concentrated in vacuo
5. customto afford crude product
6. customThe crude was purified by P-TLC and P-HPLC
7. additiontreated with a 1N solution of HCl in ether
8. customfreeze-dried