反应详情

Title compound was prepared following general procedure 1 starting from Intermediate 12 (122 mg; 0.50 mmol) and Intermediate 1 (88 mg; 0.50 mmol). Reaction mixture was filtered over a SPE-NH2 column, washed with THF followed by evaporation of the solvent under reduced pressure. Reaction mixture was extracted with ethyl acetate and combined organic phase was washed with brine, dried over magnesium sulfate and concentrated in vacuo to give a yellow oily residue. Purification by silica column chromatography (DCM/MeOH, 98/2 then 95/5) afforded the title compound as an off-white solid. 1H NMR (DMSO, d6): δ 12.78 (s, 1H), 8.39-8.37 (m, 2H), 8.31 (s, 1H), 8.24 (dd, J=8.8, 2.2 Hz, 1H), 7.95-7.92 (m, 1H), 7.78-7.75 (m, 1H), 7.32 (d, J=8.8 Hz, 1H), 4.23-4.22 (m, 1H), 3.38-3.35 (m, 2H), 1.82-1.57 (m, 6H), 1.17 (d, 6.6 Hz, 3H). HPLC (Method A) Rt 3.65 min (Purity: 95.1%). LC/MS (method B): 358.3 (M+H)+.

1. customTitle compound was prepared
2. customReaction mixture
3. filtrationwas filtered over a SPE-NH2 column
4. washwashed with THF
5. customfollowed by evaporation of the solvent under reduced pressure
6. customReaction mixture
7. extractionwas extracted with ethyl acetate and combined organic phase
8. washwas washed with brine
9. dry with materialdried over magnesium sulfate
10. concentrationconcentrated in vacuo
11. customto give a yellow oily residue
12. customPurification by silica column chromatography (DCM/MeOH, 98/2