反应详情

A mixture of Intermediate 37G (255 mg, 0.466 mmol) in 33% HBr in HOAc (1149 μl, 6.98 mmol) was stirred at room temperature for 1 h. Ether was added and the resulting solid precipitate was collected by filtration and rinsed with ether. The solid was dissolved in MeOH (10 mL) and K2CO3 (1.3 g) was added. The mixture was stirred for 40 min. and then filtered and concentrated to dryness to afford Intermediate 37H (133 mg). HPLC: RT=1.102 min (CHROMOLITH® SpeedROD column 4 6×50 mm, 10-90% aqueous methanol over 4 minutes containing 0.1% TFA, 4 mL/min, monitoring at 220 nm), MS(ES): m/z=300.2 [M+H+].

1. filtrationthe resulting solid precipitate was collected by filtration
2. washrinsed with ether
3. dissolutionThe solid was dissolved in MeOH (10 mL)
4. additionK2CO3 (1.3 g) was added
5. stirringThe mixture was stirred for 40 min.
6. filtrationfiltered
7. concentrationconcentrated to dryness