反应详情

20.08 g (0.08 mole) of methyl (2S,3R)-2-(N-benzoyl amino)methyl-3-hydroxybutyrate were dissolved in 60.8 g of 12N-hydrochloric acid solution, refluxed with application of heat for 6 hours and cooled to room temperature, so that a solid was precipitated. After the solid was filtered, the filtrate was washed twice with 100 ml of toluene. Then a water phase was concentrated to a residue in vacuo. To this was added 250 ml of acetonitrile and further, under an ice water cooling, 0.08 g (0.08 mole) of triethylamine. The total solution was stirred overnight at room temperature to yield precipitates. The precipitates were filtered, washed with 200 ml of acetonitrile and dried in vacuo, thereby obtaining 8.51 g (0.06 mole) of (2S,3R)-2-aminomethyl-3-hydroxybutyric acid. Yield was 80%. This compound corresponded to that described in the Japanese published application Hei 2-134 349 according to an 1H-NMR spectrum analysis.

1. temperaturerefluxed with application
2. temperatureof heat for 6 hours
3. customwas precipitated
4. filtrationAfter the solid was filtered
5. washthe filtrate was washed twice with 100 ml of toluene
6. concentrationThen a water phase was concentrated to a residue in vacuo
7. additionTo this was added 250 ml of acetonitrile
8. customto yield
9. customprecipitates
10. filtrationThe precipitates were filtered
11. washwashed with 200 ml of acetonitrile
12. customdried in vacuo