反应详情

温度

25 °C

70 ml of dimethylsulfoxide were added over 10 minutes at 60°-65° C. to a mixture of 20 ml of dimethylsulfoxide and 9.2 g of sodium hydride in a 50% oil disperson and after cooling the mixture to 25° C., 17.28 g of N,N-dimethyl-3-phenyl-3-hydroxy-propanamine were added thereto. The temperature returned to room temperature and 25.2 g of o-chloro-nitrobenzene were added thereto. The mixture was held at 25° C. for one hour and was then extracted with ethyl acetate. The organic phase was washed with water, dried and evaporated to dryness to obtain 41 g of raw product which was taken up twice in 100 ml of N hydrochloric acid. The neutral fraction was extracted twice with 400 ml of ether and the aqueous phase was made alkaline by addition of 50 ml of sodium hydroxide solution. The mixture was extracted with methylene chloride and the organic phase was washed with water, dried and treated with activated carbon. The mixture was filtered and the filtrate was evaporated to dryness to obtain 22 g of N,N-dimethyl-γ-(2-nitrophenoxy)-benzene-propanamine.

1. customreturned to room temperature
2. extractionwas then extracted with ethyl acetate
3. washThe organic phase was washed with water
4. customdried
5. customevaporated to dryness
6. customto obtain 41 g of raw product which
7. extractionThe neutral fraction was extracted twice with 400 ml of ether
8. additionby addition of 50 ml of sodium hydroxide solution
9. extractionThe mixture was extracted with methylene chloride
10. washthe organic phase was washed with water
11. customdried
12. additiontreated with activated carbon
13. filtrationThe mixture was filtered
14. customthe filtrate was evaporated to dryness