反应详情

温度

25 °C

Suspend lithium aluminum hydride (0.359 g, 9.46 mmol) in tetrahydrofuran (25 mL) at −10° C. and add 3,5-dimethyl-1-pyridin-2-yl-1H-pyrazole-4-carboxylic acid ethyl ester (1.160 g, 4.73 mmol) dropwise in tetrahydrofuran (5 mL). Allow the mixture to warm to 25° C. and stir for 4 hr. Cool the mixture to 0° C. then quench carefully with saturated sodium sulfate solution (1 mL). Allow the mixture to stir at room temperature for 2 hr. then filter off the precipitate, dry the solution and concentrate to give (3,5-dimethyl-1-pyridin-2-yl-1H-pyrazol-4-yl)-methanol as a yellow solid (0.821 g, 86%). 1H-NMR (400 MHz, DMSO) 8.408 (m, 1H); 7.889 (m, 1H); 7.738 (m, 1H); 7.256 (m, 1H); 4.269 (s, 2H); 2.459 (s, 3H); 2.181 (s, 3H)

1. customat −10° C.
2. temperatureCool the mixture to 0° C.
3. customthen quench carefully with saturated sodium sulfate solution (1 mL)
4. stirringAllow the mixture to stir at room temperature for 2 hr
5. filtrationthen filter off the precipitate
6. customdry the solution
7. concentrationconcentrate