反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 100 °C
PROCEDURE
实验过程
N-[2-(2-methylamino-2-phenylethyl)phenyl]-2,2-dimethyl-propanamide (155 g, 0.5 mol) was dissolved in 6 N 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-phenylphenethylamine 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
- temperatureThe reaction mixture was cooled to 23° C.
- stirringStirring
- customhad crystallized from the aqueous phase
- filtrationThe product was collected by filtration
- washwashed with toluene (2×50 ml)
- customdried in vacuo (30 mm) at 60° C. for 60 hours