反应详情

温度

35 °C

To a 3 gallon tank is added tert-butyl 4-(5-(2-fluoro-4-nitrophenoxy)-1-methyl-1H-indazol-6-yl)-1H-pyrazole-1-carboxylate (433.0 g, 952.8 mmol) followed by THF (6.5 L) and Pd/C (21.65 g, 10% Pd/C and 21.65 g, 5% Pd/C). The mixture is heated to 35° C. under hydrogen gas for 2 hours. The reaction is then cooled to RT and allowed to stir under hydrogen gas overnight, then is heated to 40° C. under hydrogen gas for seven hours. An additional 2 g Pd/C (1 g, 10% Pd/C and 1 g, 5% Pd/C) is added and stirred under hydrogen gas for another hour and cooled to RT. The mixture is again stirred under hydrogen gas overnight and the reaction is completed. The mixture is filtered over a combination of GFF® and Watman® paper. The filtrate is concentrated to a slightly yellow solid (446 g, 110% recovery).

1. temperatureThe reaction is then cooled to RT
2. temperatureis heated to 40° C. under hydrogen gas for seven hours
3. stirringstirred under hydrogen gas for another hour
4. temperaturecooled to RT
5. stirringThe mixture is again stirred under hydrogen gas overnight
6. filtrationThe mixture is filtered over a combination of GFF® and Watman® paper
7. concentrationThe filtrate is concentrated to a slightly yellow solid (446 g, 110% recovery)