HRID656800

反应详情

EQUATION

反应方程式

HRID 656800 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 153.9 g (1.12 mol) of 2-nitrotoluene in 900 ml of DMF are added, within one hour, 4.5 g (80.2 mmol) of KOH and simultaneously 193.3 g (2.24 mol) of pivalaldehyde. Subsequently, first a further 0.5 equivalent of pivalaldehyde is added and the mixture is stirred at RT for one hour, then another 0.5 equivalent of pivalaldehyde is added and the mixture is stirred at room temperature for a further 2 hours. The mixture is acidified with 40 ml of 10 percent aqueous hydrochloric acid until the color changes (pH 4.5) and a majority of the DMF is distilled off under reduced pressure. After the residue has been distilled at 130° C./0.9 mbar, 136.8 g (yield 54% of theory, purity (GC-MS 98%) of 3,3-dimethyl-1-(2-nitrophenyl)butan-2-ol are obtained.

WORKUP

后处理

  1. stirringthe mixture is stirred at room temperature for a further 2 hours
  2. distillationa majority of the DMF is distilled off under reduced pressure
  3. distillationAfter the residue has been distilled at 130° C./0.9 mbar, 136.8 g (yield 54% of theory, purity (GC-MS 98%) of 3,3-dimethyl-1-(2-nitrophenyl)butan-2-ol
  4. customare obtained