HRID656802

反应详情

EQUATION

反应方程式

HRID 656802 的结构方程式

AUXILIARIES

t.reaction.reagentsCatalystsSolvents

2

PROCEDURE

实验过程

3 g (13.4 mmol) of 3,3-dimethyl-1-(2-nitrophenyl)butan-2-ol are stirred in 50 ml of THF with 2.06 g of 65 percent sulfuric acid and 0.214 g of palladium/carbon (10%) at 90° C. under 10 bar of hydrogen pressure for 16 hours. Subsequently, the solution is filtered with suction through Celite and the filtrate is concentrated by rotary evaporation. After dissolution in ethyl acetate, washing with saturated sodium bicarbonate solution, and removal and concentration of the organic phase under reduced pressure, 2.2 g (75% of theory) of a solid are obtained. Purity (GC-MS): 88%.

WORKUP

后处理

  1. filtrationSubsequently, the solution is filtered with suction through Celite
  2. concentrationthe filtrate is concentrated by rotary evaporation
  3. dissolutionAfter dissolution in ethyl acetate
  4. washwashing with saturated sodium bicarbonate solution, and removal and concentration of the organic phase under reduced pressure, 2.2 g (75% of theory) of a solid
  5. customare obtained