反应详情

温度

0 °C

A solution of N-{4-[4-(3-bromo-4-fluorophenyl)-5-oxo-4,5-dihydro-1,2,4-oxadiazol-3-yl]-1,2,5-oxadiazol-3-yl}-1H-tetrazole-5-carboxamide (12 mg, 27 μmol) in pyridine (0.3 mL) was treated with phosphorus pentachloride (13 mg, 60 μmol) at 25° C. The reaction mixture was stirred at 0° C. for 2 h, concentrated, rediluted with toluene and concentrated to a residue. This material was diluted with ethanol (1 mL), treated with sodium cyanoborohydride (5 mg, 82 μmol), and stirred for 2 h. The reaction mixture was concentrated, diluted with ethanol (1 mL), treated with 2.0 M sodium hydroxide in water (0.2 mL), and stirred for 45 min. Purification of the crude reaction mixture by preparative LCMS gave the desired product (2 mg, 19%). LCMS for C11H10BrFN9O2 (M+H)+: m/z=398.0, 400.0.

1. concentrationconcentrated
2. additionrediluted with toluene
3. concentrationconcentrated to a residue
4. additionThis material was diluted with ethanol (1 mL)
5. stirringstirred for 2 h
6. concentrationThe reaction mixture was concentrated
7. additiondiluted with ethanol (1 mL)
8. additiontreated with 2.0 M sodium hydroxide in water (0.2 mL)
9. stirringstirred for 45 min
10. customPurification of the crude
11. customreaction mixture by preparative LCMS