反应详情

To a suspension of sodium thiomethoxide (0.806 g, 11.5 mmol) in THF (40 ml) at 0° C. was added 1B (1.368 g, 7.66 mmol) in THF (25 ml). The mixture was stirred at room temperature for 1.5 h. The reaction mixture was concentrated to about 15 ml, and water (100 ml) was added. The slurry was stirred at 0° C. for 30 min. The solid was collected by filtration, washed with water and dried to give 1C (1.209 g, 83%) as a solid. The compound has an analytical HPLC retention time=1.899 min (Chromolith SpeedROD column 4.6×50 mm, 10-90% aqueous methanol containing 0.1% TFA over 4 minutes, 4 mL/min, monitoring at 254 nm) and a LC/MS M++H=191+.

1. concentrationThe reaction mixture was concentrated to about 15 ml, and water (100 ml)
2. additionwas added
3. stirringThe slurry was stirred at 0° C. for 30 min
4. filtrationThe solid was collected by filtration
5. washwashed with water
6. customdried