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A mixture of III (125 g - 0.6 mole), acetic anhydride (214 g - 2.1 moles), Raney Nickel (1.2 ml) and acetic acid (36 g - 0.6 mole) was hydrogenated at 80° C and a pressure of 100 to 30 atm. Reaction time: 5 hours. After cooling, the catalyst was filtered, the filtrate was concentrated by normal pressure until 135 ml of distillate were collected. 150 ml of H2SO4 6N were added to the residue. The reaction was very exothermic. The solution was refluxed with active carbon for 15 min. and filtered. The filtrate was mixed with 1.2 kg of ice and exactly neutralized with 2N NaOH. The precipitate was washed with water and dried at 100° C.

1. customwas hydrogenated at 80° C
2. customReaction time
3. custom5 hours
4. temperatureAfter cooling
5. filtrationthe catalyst was filtered
6. concentrationthe filtrate was concentrated by normal pressure until 135 ml of distillate
7. customwere collected
8. addition150 ml of H2SO4 6N were added to the residue
9. temperatureThe solution was refluxed with active carbon for 15 min.
10. filtrationfiltered
11. additionThe filtrate was mixed with 1.2 kg of ice
12. washThe precipitate was washed with water
13. customdried at 100° C.