反応 #1747863

反応方程式

potassium tert-butoxide

10-phenylphenothiazine-3-carbaldehyde

diethyl[4′-(diethoxyphosphorylmethyl)biphenyl-4-ylmethyl]phosphonate

→

10-Phenyl-3-(2-{4′-[2-(10-phenylphenothiazin-3-yl)vinyl]biphenyl-4-yl}vinyl)phenothiazine

溶媒

dimethyl sulfoxide

反応条件

後処理

1. 1
   その他dried over molecular sieve
2. 2
   workup.ADDITIONthe reaction solution was diluted with 200 ml of methanol
3. 3
   workup.STIRRINGstirred for a further 15 min
4. 4
   ろ過The precipitate was filtered off
5. 5
   洗浄washed with 500 ml of methanol
6. 6
   その他dried at 35° C. under reduced pressure
7. 7
   その他The crude product (5.85 g) was recrystallized in 400 ml of toluene
8. 8
   その他were obtained

実験手順

2.73 g (24.1 mmol) of potassium tert-butoxide and then 7.80 g (25.7 mmol) of 10-phenylphenothiazine-3-carbaldehyde were added under nitrogen at room temperature with stirring to a solution of 4.83 g (10.7 mmol) of diethyl[4′-(diethoxyphosphorylmethyl)biphenyl-4-ylmethyl]phosphonate in 80 ml of dimethyl sulfoxide dried over molecular sieve. After stirring at room temperature for four hours, the reaction solution was diluted with 200 ml of methanol and stirred for a further 15 min. The precipitate was filtered off, washed with 500 ml of methanol and dried at 35° C. under reduced pressure. The crude product (5.85 g) was recrystallized in 400 ml of toluene. 3.85 g of yellow solid having a melting point of 278-290° C. were obtained.

出典