Sodium Sulfate → HCID 59637282, compound

Participants

Reaction Steps

LAH (4.7 g, 0.12 mol) was charged into a flask. THF (250 mL) was added at 0° C. Then a solution of 1-(4-methoxybenzyl)-3-(trifluoromethyl)-1H-pyrazole-5-carboxamide (37 g, 0.12 mol) in THF (120 mL) was added drop wise for 30 min at 0° C. and reaction mixture was heated to reflux for 5 h. Progress of the reaction was monitored by TLC (50% ethyl acetate/hexane, Rf˜0.2). As the reaction was not completed, LAH (2.3 g) was added again and the mixture was refluxed for another 4 h. After completion of the reaction, the reaction contents were slowly added to saturated sodium sulfate (1 L) solution and filtered over celite and the product was extracted with ethyl acetate (2×500 mL). The combined extract was dried over sodium sulfate and concentrated under reduced pressure to obtain the crude (1-(4-methoxybenzyl)-3-(trifluoromethyl)-1H-pyrazol-5-yl)methanamine as an off white solid (32.5 g, crude). The crude product obtained was directly used for the next step.

Provenance & Evidence