Réaction #1747860

Équation de réaction

potassium tert-butoxide

10-phenylphenothiazine-3,7-dicarbaldehyde

diethyl benzhydrylphosphonate

→

3,7-Bis(2,2-diphenylvinyl)-10-phenylphenothiazine

Conditions de réaction

Traitement

1. 1
   Autreprepared analogously to Example 13 in U.S
2. 2
   Séchage5,130,603) in 121 ml of dimethyl sulfoxide dried over molecular sieve
3. 3
   workup.ADDITIONthe reaction solution was diluted with 1500 ml of methanol
4. 4
   workup.STIRRINGstirred for a further 15 min
5. 5
   FiltrationThe precipitate was filtered off
6. 6
   Lavagewashed with methanol
7. 7
   Autredried at 80° C. under reduced pressure
8. 8
   Autrewere obtained

Mode opératoire

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.

Source