反应详情

To a suspension of 500 mg of the above 7-[2-(3-chloro-pyridin-2-yl)-5-(2,2,2-trifluoro-ethoxy)-2H-pyrazol-3-yl]-5-methyl-1H-8-oxa-1,2,6-triaza-cyclopenta[a]naphthalen-9-one in 10 mL of acetonitrile/water (4:1, v/v) is added 885 μL (10.4 mmol) of isopropylamine. The reaction mixture is stirred for 16 hours at ambient temperature and then concentrated in vacuo. The residue is taken-up with brine and ethyl acetate. The phases are separated and the aqueous layer is washed with ethyl acetate. The combined organic layers are washed with brine, dried over MgSO4 and concentrated in vacuo. Purification of the residue by flash chromatography (SiO2, hexane/ethyl acetate 4:6) affords 60 mg (10% over two steps) of the product as a white solid; LC/MS:536/538 (M+H)+, m.p.: 247-250° C.

1. concentrationconcentrated in vacuo
2. customThe phases are separated
3. washthe aqueous layer is washed with ethyl acetate
4. washThe combined organic layers are washed with brine
5. dry with materialdried over MgSO4
6. concentrationconcentrated in vacuo
7. customPurification of the residue by flash chromatography (SiO2, hexane/ethyl acetate 4:6)