反应详情

L-isoleucine (105 g) was added to 6N-hydrochloric acid (1 l), followed by agitating the mixture, cooling it with ice, adding sodium nitrite (80 g), agitating the mixture at 0° C. for 3 hours, adding ether (300 ml), separating the resulting organic layer, extracting the aqueous layer with ether (150 ml), combining the organic layers, drying over MgSO4, distilling off ether and distilling the residue under reduced pressure, to obtain (2S,3S)-2-chloro-3-methylvaleric acid (34.2 g, b.p. 96-97/4 mmHg).

1. temperaturecooling it with ice
2. stirringagitating the mixture at 0° C. for 3 hours
3. customseparating the resulting organic layer
4. extractionextracting the aqueous layer with ether (150 ml)
5. dry with materialdrying over MgSO4
6. distillationdistilling off ether
7. distillationdistilling the residue under reduced pressure