反应详情

温度

60 °C

To a mixture of 500 mg of the above 7-[2-(3-chloro-pyridin-2-yl)-5-methoxy-2H-pyrazol-3-yl]-5-methyl-1H-8-oxa-1,2,6-triaza-cyclopenta[a]naphthalen-9-one in 10 mL of 4:1 (v/v) mixture of acetonitrile/water is added 1.0 mL (12.2 mmol) of isopropylamine. The reaction mixture is stirred during 1 hour at ambient temperature and for 2.5 hours at 60° C. and then concentrated in vacuo. The residue is taken-up with brine and tert-butylmethylether. The phases are separated and the aqueous layer is washed with tert-butylmethylether. The combined organic layers are washed with brine, dried over MgSO4 and concentrated in vacuo. Purification of the residue by flash chromatography (SiO2, hexanes/ethyl acetate 3:7) affords 118 mg (19% over two steps) of the product as white solid; LC/MS:468/470 (M+H)+, m.p.: 148-151° C.

1. concentrationconcentrated in vacuo
2. customThe phases are separated
3. washthe aqueous layer is washed with tert-butylmethylether
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, hexanes/ethyl acetate 3:7)