反应详情

温度

50 °C

A mixture of 770 mg of 4-benzyloxy-3-(N-tert-butoxycarbonyl-N-methylsulfonylamino)-1-((2S)2,3-epoxypropoxy)benzene (1.71 mmol) and 300 mg (1.8 mmol) of 1,2,3,4-tetrahydronaphthalen-2-ylmethylamine, obtained as described in EP-A-436435, in 20 ml of absolute ethanol is heated under reflux for 16 hours. The mixture is cooled, 3 ml of an ethanol solution saturated with hydrochloric acid are added thereto and the medium is heated at 50° C. for 5 hours. The solvent is evaporated and the medium is taken up with a mixture of 50 ml of a saturated sodium bicarbonate solution and 50 ml of ethyl acetate. The organic phase is washed with a saturated aqueous NaCl solution. The organic phase is dried, filtered and the solvent is evaporated under reduced pressure. The crude product is purified by chromatography on a silica gel column, eluting with a methylene chloride/methanol=95/5 mixture. The title compound is obtained in the form of a glassy solid.

1. customobtained
2. temperatureis heated
3. temperatureunder reflux for 16 hours
4. temperatureThe mixture is cooled
5. customThe solvent is evaporated
6. additionthe medium is taken up with a mixture of 50 ml of a saturated sodium bicarbonate solution and 50 ml of ethyl acetate
7. washThe organic phase is washed with a saturated aqueous NaCl solution
8. customThe organic phase is dried
9. filtrationfiltered
10. customthe solvent is evaporated under reduced pressure
11. customThe crude product is purified by chromatography on a silica gel column
12. washeluting with a methylene chloride/methanol=95/5 mixture