反应详情

To a stirred solution of Intermediate 340A (7.0 g, 14.13 mmol) in 1,4-dioxane (10 mL) was added 4 M HCl in dioxane (25 mL, 100 mmol) and the solution was stirred at RT for 2 h. The reaction mixture was concentrated and the residue was diluted with EtOAc (20 mL). The EtOAc solution was washed successively with water, a saturated aq. solution of NaHCO3, and brine. The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure. The residue obtained was heated in a ROTAVAPOR® at 60° C. for 5 h. The solid product was washed with ether to afford Intermediate 340B (4.0 g, 87%). MS(ES): m/z=350 [M+H]+; 1H NMR (300 MHz, DMSO-d6) δ ppm 8.49 (s, 1H), 4.27-4.49 (m, 1H), 4.11-4.26 (m, 2H), 4.03 (d, J=11.71 Hz, 2H), 1.06-1.39 (m, 6H).

1. concentrationThe reaction mixture was concentrated
2. additionthe residue was diluted with EtOAc (20 mL)
3. washThe EtOAc solution was washed successively with water
4. dry with materialThe organic layer was dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated under reduced pressure
7. customThe residue obtained
8. temperaturewas heated in a ROTAVAPOR® at 60° C. for 5 h
9. washThe solid product was washed with ether