反应详情

To a mixture of methyl 3-benzyloxy-1-phenyl-1H-pyrazole-5-carboxylate (14.53 g) and tetrahydrofuran (300 ml) was slowly added aluminum lithium hydride (1.79 g) at 0° C. and the mixture was stirred at room temperature for 1 hr. Sodium sulfate 10 hydrate (15.20 g) was slowly added to the reaction mixture at 0° C. and the mixture was stirred at room temperature for 30 min. Insoluble materials were filtered off and the filtrate was concentrated. The residue was subjected to silica gel column chromatography, and (3-benzyloxy-1-phenyl-1H-pyrazol-5-yl)methanol (11.65 g, yield 88%) was obtained as colorless crystals from a fraction eluted with ethyl acetate-hexane (1:2, volume ratio). The crystals were recrystallized from ethyl acetate-hexane. melting point: 87–88° C.

1. customat 0° C.
2. stirringthe mixture was stirred at room temperature for 30 min
3. filtrationInsoluble materials were filtered off
4. concentrationthe filtrate was concentrated