反应详情

温度

0 °C

HCl (4M in dioxane, 30 mL) was added to a sol. of compound C5 (3.34 g, 4.20 mmol) in CH2Cl2 (30 mL) at 0° C. The mixture was stirred for 1 h at 0° C., then for 1 h at rt. The solvents were removed under reduced pressure, and the residue was dried under high vacuum. The residue was dissolved in CH2Cl2 (30 mL), and DIPEA (2.88 mL, 16.8 mmol) was added. The mixture was cooled to −20° C., and AcCl (0.315 mL, 4.41 mmol) was added carefully. The mixture was stirred for 20 min at −20° C., and CH2Cl2 was added. The mixture was washed with aq. 1M HCl and aq. 1M NaOH. The org. layer was dried over MgSO4, filtered, and the solvents were removed under reduced pressure. Purification of the residue by FC (EtOAc/heptane 1:4→1:3→1:2) yielded the title compound (3.03 g, 98%). LC-MS: tR=1.18 min; ES+: 738.14.

1. waitfor 1 h at rt
2. customThe solvents were removed under reduced pressure
3. customthe residue was dried under high vacuum
4. dissolutionThe residue was dissolved in CH2Cl2 (30 mL)
5. temperatureThe mixture was cooled to −20° C.
6. stirringThe mixture was stirred for 20 min at −20° C.
7. washThe mixture was washed with aq. 1M HCl and aq. 1M NaOH
8. dry with materiallayer was dried over MgSO4
9. filtrationfiltered
10. customthe solvents were removed under reduced pressure
11. customPurification of the residue by FC (EtOAc/heptane 1:4→1:3→1:2)