反应详情

1.53 g (7.90 mmol) of the compound from Example 2A and 2.92 g (23.7 mmol) of the compound from Example 1A are dissolved 2 ml anhydrous ethanol under argon and the mixture is stirred at RT for 16 h. 537 g (7.90 mmol) sodium ethanolate are added, the reaction solution becoming dark red in color. The mixture is subsequently stirred at RT for 30 min and 7.9 ml 1 M hydrochloric acid are then added. The solution is partly concentrated, a precipitate separating out. This is filtered off, washed with water (twice with 5 ml each time) and with MTBE (5 ml) and dried in vacuo. 435 mg (22% of th.) of the title compound are obtained.

1. stirringThe mixture is subsequently stirred at RT for 30 min
2. concentrationThe solution is partly concentrated
3. customa precipitate separating out
4. filtrationThis is filtered off
5. washwashed with water (twice with 5 ml each time) and with MTBE (5 ml)
6. customdried in vacuo