反应详情

In 120 ml of ethanol were dissolved 2.4 g of (R) (-)5[(2-amino-2-methyl)ethyl]-2-methoxybenzenesulfonamide and 1.2 g of 2-(o-ethoxyphenoxy)ethyl bromide, and the mixture was refluxed for 16 hours under heating. The solvent was distilled away, and after alkalifing the residue by the addition of 10% sodium hydroxide, and the oily material precipitated was extracted with ethyl acetate. The extract solution was washed with a saturated aqueous sodium chloride, and dried over anhydrous magnesium sulfate. The solvent was distilled away, and the residue was subjected to silica-gel column chromatography. The product was eluted with CHCl3 -methanol (9:5) to provide 1.5 g of the crude crystals of (R) (-)-5-[2-[[2-(o-ethoxyphenoxy)ethyl]amino]-2-methylethyl]-2-methoxybenzenesulfonamide, which was treated with HCl-ethanol to give a hydrochloric acid salt of (R) (-)-5-[2-[[2-(o-ethoxyphenoxy)ethyl]amino]-2-methylethyl]-2-methoxybenzenesulfonamide.

1. temperaturethe mixture was refluxed for 16 hours
2. temperatureunder heating
3. distillationThe solvent was distilled away
4. additionby the addition of 10% sodium hydroxide
5. customthe oily material precipitated
6. extractionwas extracted with ethyl acetate
7. washThe extract solution was washed with a saturated aqueous sodium chloride
8. dry with materialdried over anhydrous magnesium sulfate
9. distillationThe solvent was distilled away
10. washThe product was eluted with CHCl3 -methanol (9:5)
11. customto provide 1.5 g of the crude crystals of (R) (-)-5-[2-[[2-(o-ethoxyphenoxy)ethyl]amino]-2-methylethyl]-2-methoxybenzenesulfonamide, which