反应详情

The product from step 5 (55 mg, (0.09 mmol) was dissolved in 1 mL of CH2Cl2 and 1 mL of TFA was added dropwise. The mixture stirred for 1 hour and then concentrated to dryness. The residue was dissolved in acetonitrile and water was added and the pH was adjusted to 9 by the addition of aqueous K3PO4. The mixture was concentrated in vacuo and the solids obtained were extracted with MeOH, and then concentrated in vacuo again. The solid residue obtained was re-extracted with MeOH, filtered and the filtrate purified by preparative HPLC to provide 14 mg (30%) of the title compound. 1H-NMR (DMSO-d6) 8.35 (s, 1H), 7.61 (s, 1H), 7.58 (bs, 2H), 7.39-7.24 (m, 7H), 7.22 (s, 1H), 7.11-7.01, (m, 2H), 6.77 (d, 1H), 6.57 (d, 1H), 6.26 (d, 1H), 5.57 (s, 2H), 3.10 (m, 4H), 2.84 (m, 4H); LC-MS [M+H]+=501.2, RT=2.24 min.

1. concentrationconcentrated to dryness
2. dissolutionThe residue was dissolved in acetonitrile
3. additionwater was added
4. additionthe pH was adjusted to 9 by the addition of aqueous K3PO4
5. concentrationThe mixture was concentrated in vacuo
6. customthe solids obtained
7. extractionwere extracted with MeOH
8. concentrationconcentrated in vacuo again
9. customThe solid residue obtained
10. extractionwas re-extracted with MeOH
11. filtrationfiltered
12. customthe filtrate purified by preparative HPLC