HRID479079
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- filtrationThe solution was filtered
- washthe catalyst washed twice with 10 mL of MeOH
- concentrationconcentrated on the rotary evaporator to a volume of 80 mL
- addition15 mL of aqueous 10 N sodium hydroxide was added
- stirringstirred for 30 minutes at 5° C
- filtrationThe solid was filtered
- washwashed with water
- customdried at 40° C. in vacuum (30 in. Hg)