Reaktion #1747867
ord-3997275d56804cd7b800fc4a35bd29a2
Reaktionsgleichung
10-(4-benzyloxyphenyl)phenothiazine 5,5-dioxide
ammonium formate
→
10-(4-Hydroxyphenyl)phenothiazine 5,5-dioxide
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Filtrationthe solution was filtered
- 2EinengenThe filtrate was concentrated
- 3workup.ADDITIONafter adding 10 ml of methanol
- 4FiltrationThe solid was filtered off with suction
- 5Waschenwashed with methanol
- 6Sonstigedried at 110° C. in a vacuum
- 7Sonstigedrying cabinet
- 8Sonstigewere obtained
Vorschrift
3.10 g (7.50 mmol) of 10-(4-benzyloxyphenyl)phenothiazine 5,5-dioxide, 2.30 g (35.7 mmol) of 98% ammonium formate and 7.5 g of 10% palladium on activated carbon were heated to boiling under reflux in 225 ml of acetone for 1 hour. After cooling to room temperature, the solution was filtered. The filtrate was concentrated and, after adding 10 ml of methanol, stirred overnight. The solid was filtered off with suction, washed with methanol and dried at 110° C. in a vacuum drying cabinet. 1.47 g (61% of theory) of analytically pure light gray microcrystals having an m.p. of 308-311° C. were obtained.