HRID479079

反应详情

EQUATION

反应方程式

HRID 479079 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
5 °C

PROCEDURE

实验过程

2-Methylsulfonylnitrobenzene (13.0 g , 0.065 mol) was suspended in MeOH (140 mL) and 2N H2SO4 (60 mL). 6% Pd/C catalyst (50% wet; 3 g) was added to the suspension and it was hydrogenated at 40 psi in a Parr shaker for 4 hours. The solution was filtered, the catalyst washed twice with 10 mL of MeOH and concentrated on the rotary evaporator to a volume of 80 mL. The suspension was cooled to 5° C. with stirring and 15 mL of aqueous 10 N sodium hydroxide was added and stirred for 30 minutes at 5° C. The solid was filtered, washed with water and dried at 40° C. in vacuum (30 in. Hg) to give 10.5 g (95% yield) of 2-methylsulfonylaniline.

WORKUP

后处理

  1. filtrationThe solution was filtered
  2. washthe catalyst washed twice with 10 mL of MeOH
  3. concentrationconcentrated on the rotary evaporator to a volume of 80 mL
  4. addition15 mL of aqueous 10 N sodium hydroxide was added
  5. stirringstirred for 30 minutes at 5° C
  6. filtrationThe solid was filtered
  7. washwashed with water
  8. customdried at 40° C. in vacuum (30 in. Hg)