反应详情

温度

50 °C

To a round bottom flask containing 83.2B (13.15 g, 52.8 mmol) in dry DCM (90 mL) was added 3,4-dihydro-2H-pyran (10 mL, 110 mmol) followed by PPTS (0.13 g, 0.53 mmol). The reaction mixture was heated to a gentle reflux (50° C.) and monitored with TLC and LC-MS. After 24 hours, the reaction was concentrated under reduced pressure and then diluted with MeOH. After concentration, the residue was heated in a round bottom flask containing MeOH on the rotary evaporator (without vacuum.) to 40° C. After about 30 minutes, the solution was concentrated to a volume of about 5 mL. After cooling to room temperature, the white solid was filtered and rinsed once with MeOH to yield 83.2C (13.35 g, 76%). 1H NMR (400 MHz, CDCl3) δ ppm 8.25 (1H, m), 6.96 (1H, d, J=12.5 Hz), 5.56 (1H, m), 3.91 (3H, s), 3.79 (1H, td, J=11.1, 2.5 Hz), 3.65 (1H, d, J=10.6 Hz), 2.23 (2H, m), 1.96 (3H, m), 1.68 (1H, m).

1. temperatureThe reaction mixture was heated to
2. concentrationthe reaction was concentrated under reduced pressure
3. additiondiluted with MeOH
4. concentrationAfter concentration
5. temperaturethe residue was heated in a round bottom flask
6. additioncontaining MeOH
7. customon the rotary evaporator (without vacuum.) to 40° C
8. waitAfter about 30 minutes
9. concentrationthe solution was concentrated to a volume of about 5 mL
10. temperatureAfter cooling to room temperature
11. filtrationthe white solid was filtered
12. washrinsed once with MeOH