HRID247749

反应详情

EQUATION

反应方程式

HRID 247749 的结构方程式

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

N-[2-(2-methylamino-2-phenylethyl)phenyl]-2,2-dimethylpropanamide (155 g, 0.5 mol) was dissolved in 6N HCl (310 g) and stirred under a nitrogen atmosphere at 100° C. for 28 hours. The reaction mixture was cooled to 23° C. and toluene (200 ml) was added. Stirring was continued until the product had crystallized from the aqueous phase. The product was collected by filtration, washed with toluene (2×50 ml) and dried in vacuo (30 mm) at 60° C. for 60 hours to give N-methyl-2-amino-α-phenylphenethyl-amine dihydrochloride (139 g, 93% yield). The melting point of the product was 252°-254° C. The organic phase of the filtrate was concentrated in vacuo to give a 58% recovery of trimethylacetic acid. The aqueous phase of the filtrate afforded a second crop of N-methyl-2-amino-α-phenylphenethylamine dihydrochloride (9.3 g, 6%) The total yield of product was 99%.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 23° C.
  2. stirringStirring
  3. customhad crystallized from the aqueous phase
  4. filtrationThe product was collected by filtration
  5. washwashed with toluene (2×50 ml)
  6. customdried in vacuo (30 mm) at 60° C. for 60 hours