反应详情

温度

42.5 °C

To a solution of (S)-2-({3-[4-(6-Fluoro-benzothiazol-2-ylamino)-phenyl]-N-hydroxy-isoxazole-5-carboximidoyl}-amino)-3-methyl-butyric acid methyl ester (0.3 g; 0.62 mmol) in THF (3 ml) was added 1N LiOH (0.81 ml; 0.81 mmol) under stirring for 48 hours, followed by heating at 40-45° C. for 2 hours. Solvent was removed from the reaction mixture and the residue was diluted with water (5 ml) and acidified to pH 2 with 2N HCl. The semisolid material obtained was extracted with EtOAc, washed with water (2×5 ml), and dried over anhydrous Na2SO4. The residue was purified by flash chromatography with 10-50% MeOH in chloroform. The pure material obtained was triturated with acetone and light petroleum, filtered and dried under vacuum pump to yield 0.16 g (55%) of the title compound. Mass

1. customSolvent was removed from the reaction mixture
2. additionthe residue was diluted with water (5 ml)
3. customThe semisolid material obtained
4. extractionwas extracted with EtOAc
5. washwashed with water (2×5 ml)
6. dry with materialdried over anhydrous Na2SO4
7. customThe residue was purified by flash chromatography with 10-50% MeOH in chloroform
8. customThe pure material obtained
9. customwas triturated with acetone and light petroleum
10. filtrationfiltered
11. customdried under vacuum pump