反应 #1747870

ord-503147315ea649f08e5d68cb04c58034

反应方程式

c1ccc(-n2c(-c3ccc(N4c5ccccc5Sc5ccccc54)cc3)nc3ccccc32)cc1
10-[4-(N-phenyl-2-benzimidazolyl)phenyl]phenothiazine
O=C(OO)c1cccc(Cl)c1
m-chloroperbenzoic acid
[K+].[OH-]
KOH
O=S1(=O)c2ccccc2N(c2ccc(-c3nc4ccccc4n3-c3ccccc3)cc2)c2ccccc21
10-[4-(N-Phenyl-2-benzimidazolyl)phenyl]phenothiazine 5,5-dioxide

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度with cooling
  2. 2
    其他After the methylene chloride had been removed
  3. 3
    workup.ADDITIONthe suspension was diluted with 100 ml of hot water
  4. 4
    过滤The precipitate was filtered off with suction
  5. 5
    洗涤washed with hot water
  6. 6
    其他dried at 80° C. under reduced pressure
  7. 7
    其他The crude product (4.82 g) was recrystallized from 48 ml of acetic acid
  8. 8
    其他were obtained

实验过程

A solution of 6.14 g of 10-[4-(N-phenyl-2-benzimidazolyl)phenyl]phenothiazine in 180 ml of methylene chloride was admixed at room temperature with 7.17 g (28.9 mmol) of 70% m-chloroperbenzoic acid with cooling and stirred at room temperature for 1 h. The solution was admixed with 60 ml of 10% KOH. After the methylene chloride had been removed, the suspension was diluted with 100 ml of hot water. The precipitate was filtered off with suction, washed with hot water and dried at 80° C. under reduced pressure. The crude product (4.82 g) was recrystallized from 48 ml of acetic acid. 3.02 g (46% of theory) of beige microcrystals having an m.p. of 286-288° C. were obtained.

来源

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