反应 #1747860
ord-a9d196f96d29410e8f8136439c0d4ad2
反应方程式
potassium tert-butoxide
10-phenylphenothiazine-3,7-dicarbaldehyde
diethyl benzhydrylphosphonate
→
3,7-Bis(2,2-diphenylvinyl)-10-phenylphenothiazine
反应条件
详细条件
See reaction.notes.procedure_details.
后处理
- 1其他prepared analogously to Example 13 in U.S
- 2干燥5,130,603) in 121 ml of dimethyl sulfoxide dried over molecular sieve
- 3workup.ADDITIONthe reaction solution was diluted with 1500 ml of methanol
- 4workup.STIRRINGstirred for a further 15 min
- 5过滤The precipitate was filtered off
- 6洗涤washed with methanol
- 7其他dried at 80° C. under reduced pressure
- 8其他were obtained
实验过程
6.63 g (58.1 mmol) of potassium tert-butoxide and then 8.50 g (25.7 mmol) of 10-phenylphenothiazine-3,7-dicarbaldehyde were added at room temperature with stirring to a solution of 15.61 g (51.3 mmol) of diethyl benzhydrylphosphonate (prepared analogously to Example 13 in U.S. Pat. No. 5,130,603) in 121 ml of dimethyl sulfoxide dried over molecular sieve. After stirring at room temperature for 5 hours, the reaction solution was diluted with 1500 ml of methanol and stirred for a further 15 min. The precipitate was filtered off, washed with methanol and dried at 80° C. under reduced pressure. 6.92 g (43% of theory) of yellowish solid having a melting point of 232-237° C. were obtained.