反应详情

210 mg (0.19 mmol, purity 61%) of the compound from Example 47A were stirred in 4.4 ml of a 25% strength solution of trifluoroacetic acid in methylene chloride at RT for 30 min. The mixture was then concentrated under reduced pressure. The residue was dissolved in a little methanol and added to semiconcentrated aqueous sodium bicarbonate solution. After 15 min of stirring at RT, 15 ml of ethyl acetate were added. The precipitate formed was filtered off, and the organic phase of the filtrate was separated off, washed with water, dried over sodium sulphate, filtered and concentrated. Drying of the residue under reduced pressure gave 41 mg (37% of theory) of the title compound.

1. concentrationThe mixture was then concentrated under reduced pressure
2. dissolutionThe residue was dissolved in a little methanol
3. additionadded to semiconcentrated aqueous sodium bicarbonate solution
4. addition15 ml of ethyl acetate were added
5. customThe precipitate formed
6. filtrationwas filtered off
7. customthe organic phase of the filtrate was separated off
8. washwashed with water
9. dry with materialdried over sodium sulphate
10. filtrationfiltered
11. concentrationconcentrated
12. customDrying of the residue under reduced pressure