HRID875294

反应详情

EQUATION

反应方程式

HRID 875294 的结构方程式

PROCEDURE

实验过程

In a three-neck flask, at 20° C. and under an inert atmosphere, are mixed ethyl 2-hydroxyvalerate (31 g; 210 mmol) and sodium methylate in solution in methanol (25% w/w) (2.2 g; 10 mmol). To this mixture, is added dimethylamine in solution in methanol (50% w/w) (37.1 g; 411 mmol) within 30 minutes. The temperature of this mixture is brought to 40° C. and maintained for 3 hours. After return of the temperature of the reaction mixture to 20° C., orthophosphonic acid is added until a pH of 5 is obtained. The salts formed are removed by filtration and the solvents are removed under reduced pressure. 2-hydroxy-N,N-dimethylhexanamide is then obtained with a purity <98% i.e. a yield of 80%.

WORKUP

后处理

  1. customis brought to 40° C.
  2. temperaturemaintained for 3 hours
  3. additionAfter return of the temperature of the reaction mixture to 20° C., orthophosphonic acid is added until a pH of 5
  4. customis obtained
  5. customThe salts formed
  6. customare removed by filtration
  7. customthe solvents are removed under reduced pressure