反应详情

240 mg (854 μmol) of the compound from Example 2A, 150 mg (776 mmol) of the compound from Example 8A and 18 mg (78 μmol) camphor-10-sulfonic acid are dissolved in 3 ml anhydrous ethanol and the mixture is heated under reflux overnight. After cooling, 64 mg (931 μmol) sodium ethylate are added and the mixture is further stirred overnight at RT. The precipitate formed is filtered off with suction, washed with ethanol and diethyl ether and dried. The filtrate is concentrated and the residue is purified by means of preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient). The two intermediate product fractions obtained in this way are suspended together in 5 ml methanol, 15 mg (278 μmol) sodium methylate are added and the mixture is heated under reflux overnight. After cooling, the reaction mixture is purified by means of preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient) and 26 mg (8% of th.) of the title compound are obtained.

1. temperaturethe mixture is heated
2. temperatureunder reflux overnight
3. temperatureAfter cooling
4. customThe precipitate formed
5. filtrationis filtered off with suction
6. washwashed with ethanol and diethyl ether
7. customdried
8. concentrationThe filtrate is concentrated
9. customthe residue is purified by means of preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient)
10. customThe two intermediate product fractions obtained in this way
11. temperaturethe mixture is heated
12. temperatureunder reflux overnight
13. temperatureAfter cooling
14. customthe reaction mixture is purified by means of preparative HPLC (RP18 column; mobile phase: acetonitrile/water gradient) and 26 mg (8% of th.) of the title compound
15. customare obtained