HRID2288133

反应详情

EQUATION

反应方程式

HRID 2288133 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

0.01 g of ammonium vanadate and 5 g of titanium dioxide extrudate containing 1% by weight of metallic palladium and having a particle size of 3 mm (from Johnson Matthey) are added to a suspension consisting of 500 ml of water and 19.3 g of 5-methyl-6-nitrobenzimidazolone. After displacing the air with nitrogen, the latter is replaced by hydrogen at atmospheric pressure and the suspension is stirred at 65° C. for 78 hours. During this time, 105% of the theoretical amount of hydrogen, based on the 5-methyl-6-nitrobenzimidazolone, is adsorbed. The resulting suspension is then sieved through a sieve having a mesh width of 1 mm. The material remaining on the sieve is washed with 100 ml of water and the combined aqueous phases are then filtered through a paper filter and washed with 50 ml of water. Drying at 80° C. under reduced pressure (125 mbar) gives 15.1 g (93%) of 5-amino-6-methylbenzimidazolone.

WORKUP

后处理

  1. additionare added to a suspension
  2. filtrationThe resulting suspension is then sieved through a sieve
  3. washis washed with 100 ml of water
  4. filtrationthe combined aqueous phases are then filtered through a paper
  5. filtrationfilter
  6. washwashed with 50 ml of water
  7. customDrying at 80° C. under reduced pressure (125 mbar)