反应详情

To a stirred solution of trans-4-[4-amino-5-(4-phenoxy-phenyl)-imidazo[5,1-f][1,2,4]triazin-7-yl]-cyclohexanecarboxylic acid methyl ester (105.0 mg, 0.2368 mmol) in THF (7 mL) was added solution of LiAlH4 in THF (1.0 M, 1.0 mL) at −78° C. The solution was allowed to warm to rt. Sat. aq. NaHCO3 (10 mL) was added to the reaction mixture, and the THF was removed in vacuo. DCM was added, and the mixture was transferred to a separatory funnel. The organic layer was extracted with sat. aq. NaHCO3, washed with brine, dried with magnesium sulfate, filtered and concentrated in vacuo to afford the title compound as an off-white solid. MS (ES+): m/z 416.09 (100) [MH+]. HPLC tR=3.12 min (OpenLynx, polar—5 min).

1. customthe THF was removed in vacuo
2. additionDCM was added
3. customthe mixture was transferred to a separatory funnel
4. extractionThe organic layer was extracted with sat. aq. NaHCO3
5. washwashed with brine
6. dry with materialdried with magnesium sulfate
7. filtrationfiltered
8. concentrationconcentrated in vacuo