반응 #1747867
ord-3997275d56804cd7b800fc4a35bd29a2
반응 방정식
10-(4-benzyloxyphenyl)phenothiazine 5,5-dioxide
ammonium formate
→
10-(4-Hydroxyphenyl)phenothiazine 5,5-dioxide
용매
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1여과the solution was filtered
- 2농축The filtrate was concentrated
- 3workup.ADDITIONafter adding 10 ml of methanol
- 4여과The solid was filtered off with suction
- 5세척washed with methanol
- 6기타dried at 110° C. in a vacuum
- 7기타drying cabinet
- 8기타were obtained
실험 절차
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.