反应详情

A solution of 0.6 g of the compound obtained in EXAMPLE 9 and 0.18 ml of triethylamine in 10 ml of DCM is cooled to 0° C., 0.1 ml of propionyl chloride is added dropwise and the mixture is stirred for 5 minutes. It is concentrated under vacuum, the residue is extracted with AcOEt, the organic phase is washed twice with water and dried over MgSO4 and the solvent is evaporated off under vacuum. The residue is chromatographed on silica H using DCM and then a DCM/MeOH mixture (95/5; v/v) as the eluent. The product obtained is taken up with ethereal hydrogen chloride and the precipitate formed is filtered off to give 0.37 g of the expected product.

1. concentrationIt is concentrated under vacuum
2. extractionthe residue is extracted with AcOEt
3. washthe organic phase is washed twice with water
4. dry with materialdried over MgSO4
5. customthe solvent is evaporated off under vacuum
6. customThe residue is chromatographed on silica H
7. customThe product obtained
8. customthe precipitate formed
9. filtrationis filtered off