反应详情

(3-(Trifluoromethyl)-1H-pyrazol-4-yl)methanol (54.00 g, 0.325 mol) was suspended in toluene (2 L). MnO2 (113.00 g, 1.30 mol) and 4 Å molecular sieve powder (54.00 g) were added. The reaction mixture was stirred at reflux under nitrogen with a Dean-Stark trap for 5.5 h. The resulting mixture was filtered hot and the cake allowed to cool before washing with 1:1 DCM:MeOH solution (3×500 mL). The combined filtrates were concentrated in vacuo to give the desired product (54.00 g, 0.329 mol, 100%).

1. temperatureat reflux under nitrogen with a Dean-Stark trap for 5.5 h
2. filtrationThe resulting mixture was filtered hot
3. temperatureto cool
4. washbefore washing with 1:1 DCM
5. concentrationThe combined filtrates were concentrated in vacuo