反应详情

To a slurry of 15 g. of 2-bromoethylamine hydrobromide in 150 ml. of 1,2-dimethoxyethane are added simultaneously solutions of 31 g. of 2-(4-tetradecenylamino)benzoyl chloride hydrochloride in 60 ml. of 1,2-dimethoxyethane and 50 cc. of triethylamine (dropwise). Upon addition of 0.5 g. of 4-dimethylaminopyridine the mixture is stirred at room temperature overnight. The solution is refluxed for one hour and filtered. The solid is oven dried and partitioned between methylene chloride and water. The layers are separated and the organic phase dried over magnesium sulfate. The organic layer is concentrated and the residue collected and crystallized from cyclohexane and recrystallized from acetonitrile to yield the product.

1. additionUpon addition of 0.5 g
2. temperatureThe solution is refluxed for one hour
3. filtrationfiltered
4. customdried
5. custompartitioned between methylene chloride and water
6. customThe layers are separated
7. dry with materialthe organic phase dried over magnesium sulfate
8. concentrationThe organic layer is concentrated
9. customthe residue collected
10. customcrystallized from cyclohexane
11. customrecrystallized from acetonitrile
12. customto yield the product