反応 #1747867

反応方程式

10-(4-benzyloxyphenyl)phenothiazine 5,5-dioxide

ammonium formate

→

10-(4-Hydroxyphenyl)phenothiazine 5,5-dioxide

溶媒

acetone

反応条件

後処理

1. 1
   ろ過the solution was filtered
2. 2
   濃縮The filtrate was concentrated
3. 3
   workup.ADDITIONafter adding 10 ml of methanol
4. 4
   ろ過The solid was filtered off with suction
5. 5
   洗浄washed with methanol
6. 6
   その他dried at 110° C. in a vacuum
7. 7
   その他drying cabinet
8. 8
   その他were obtained

実験手順

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.

出典