反应详情

温度

40 °C

There was dissolved, in 34 mL of methanol, 4.47 g of the crude product of 5-(N-formyl-N-methylamino-methyl)-2-nitrobenzoic acid methyl ester, prepare in the step 1, 5% Pd/C (wet product) was added to the solution in an argon gas atmosphere and then hydrogen gas was introduced into the reaction container. The reaction system was stirred at a reaction temperature of 40° C. for 8 hours, the hydrogen gas was replaced with argon gas, 14 mL of methanol was then added to the reaction system and the temperature thereof was raised up to 55° C. The Pd/C catalyst was removed through filtration under reduced pressure, the catalyst was washed with 25 mL of methanol and the resulting filtrate and the wash liquid were maintained at a temperature of 40° C. Water (31 mL) was dropwise added thereto thus separate out solid and the resulting slurry was stirred at 10° C. overnight. The resulting solid was separated from the slurry through filtration under reduced pressure, washed with 7 mL of water and then dried under reduced pressure at 70° C. for 5 hours to give 2.53 g of the title compound as a white solid.

1. additionwas added to the solution in an argon gas atmosphere
2. additionwas then added to the reaction system
3. temperaturethe temperature thereof was raised up to 55° C
4. customThe Pd/C catalyst was removed through filtration under reduced pressure
5. washthe catalyst was washed with 25 mL of methanol
6. temperaturethe resulting filtrate and the wash liquid were maintained at a temperature of 40° C
7. additionWater (31 mL) was dropwise added
8. customthereto thus separate out solid
9. stirringthe resulting slurry was stirred at 10° C. overnight
10. customThe resulting solid was separated from the slurry through filtration under reduced pressure
11. washwashed with 7 mL of water
12. customdried under reduced pressure at 70° C. for 5 hours