反应详情

A solution of 0.6 g of the compound obtained in EXAMPLE 17 and 0.5 ml of triethylamine in 25 ml of DCM is cooled to 0-5° C., 0.085 ml of acetyl chloride is added and the mixture is stirred for 3 hours, the temperature being allowed to rise to RT. It is concentrated under vacuum, the residue is taken up with water and extracted with AcOEt, the organic phase is washed with water and dried over Na2SO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica using DCM and then a DCM/MeOH mixture (98/2; v/v) as the eluent. The product obtained is dissolved in DCM and acidified by the addition of ethereal hydrogen chloride and the precipitate formed is filtered off to give 1.2 g of the expected product, m.p.=105-107° C.

1. customto rise to RT
2. concentrationIt is concentrated under vacuum
3. extractionextracted with AcOEt
4. washthe organic phase is washed with water
5. dry with materialdried over Na2SO4
6. customthe solvent is evaporated off under vacuum
7. customThe residue is chromatographed on silica
8. customThe product obtained
9. customthe precipitate formed
10. filtrationis filtered off