反应 #1747867
ord-3997275d56804cd7b800fc4a35bd29a2
反应方程式
10-(4-benzyloxyphenyl)phenothiazine 5,5-dioxide
ammonium formate
→
10-(4-Hydroxyphenyl)phenothiazine 5,5-dioxide
溶剂
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1过滤the solution was filtered
- 2浓缩The filtrate was concentrated
- 3workup.ADDITIONafter adding 10 ml of methanol
- 4过滤The solid was filtered off with suction
- 5洗涤washed with methanol
- 6其他dried at 110° C. in a vacuum
- 7其他drying cabinet
- 8其他were obtained
实验过程
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.