反应详情

温度

100 °C

A stirred suspension of methyl (2R)-2-[(4-{[1-(pyridin-2-ylmethyl)-1H-indazol-5-yl]amino}quinazolin-5-yl)oxy]propanoate (200 mg, 0.44 mmol) in 2-(methylamino)-ethanol (2 ml) was heated in a microwave reactor at 100° C. for 30 minutes. The 2-(methylamino)-ethanol was evaporated under high vacuum and the residue was partitioned between water and DCM. The organic phase was washed with brine, dried and evaporated to a gum. The title compound was isolated by chromatography (silica, 5% 2M NH3-methanol in DCM) as a white solid after trituration with ether (126 mg, 58%); NMR spectrum (393 K) 1.65 (d, 3H), 3.07 (s, 2H), 3.39-3.66 (m, 5H), 4.40 (s, 1H), 5.71 (s, 2H), 5.76-5.83 (m, 1H), 7.05 (d, 1H), 7.20 (d, 1H), 7.23-7.28 (m, 1H), 7.35 (d, 1H), 7.58 (d, 1H), 7.65-7.73 (m, 2H), 7.84 (dd, 1H), 8.07 (s, 1H), 8.45 (s, 1H), 8.48 (s, 1H), 8.52 (d, 1H), 10.86 (s, 1H); Mass spectrum MH+ 498.

1. customThe 2-(methylamino)-ethanol was evaporated under high vacuum
2. customthe residue was partitioned between water and DCM
3. washThe organic phase was washed with brine
4. customdried
5. customevaporated to a gum