反应详情

温度

70 °C

55 ml of a 1N K2CO3 solution are added dropwise to 3.12 g (5.5 mmol) of 1-[4-(thiazol-2-yl)-phenyl]-4(S)-hydroxy-2-(tert-butoxycarbonyl)amino-5(S)-(trifluoroacetyl)amino-6-phenyl-2-azahexane in 55 ml of methanol and the mixture is stirred at 70° C. for 9 hours. The mixture is cooled and ≈30 ml of methanol are evaporated off; methylene chloride and water are added and the aqueous phase is separated off and extracted with methylene chloride; the organic phases are washed with water, dried (Na2SO4) and concentrated by evaporation, yielding the title compound: HPLC20-100: tRet=1.9; FAB MS (M+H)+=469.

1. temperatureThe mixture is cooled
2. custom≈30 ml of methanol are evaporated off
3. additionmethylene chloride and water are added
4. customthe aqueous phase is separated off
5. extractionextracted with methylene chloride
6. washthe organic phases are washed with water
7. dry with materialdried (Na2SO4)
8. concentrationconcentrated by evaporation