反应 #1747860

ord-a9d196f96d29410e8f8136439c0d4ad2

反应方程式

CC(C)(C)[O-].[K+]
potassium tert-butoxide
O=Cc1ccc2c(c1)Sc1cc(C=O)ccc1N2c1ccccc1
10-phenylphenothiazine-3,7-dicarbaldehyde
CCOP(=O)(OCC)C(c1ccccc1)c1ccccc1
diethyl benzhydrylphosphonate
C(=C(c1ccccc1)c1ccccc1)c1ccc2c(c1)Sc1cc(C=C(c3ccccc3)c3ccccc3)ccc1N2c1ccccc1
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. 1
    其他prepared analogously to Example 13 in U.S
  2. 2
    干燥5,130,603) 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
    过滤The precipitate was filtered off
  6. 6
    洗涤washed with methanol
  7. 7
    其他dried at 80° C. under reduced pressure
  8. 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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08029919B2uspto-grants-2011_10