反応 #1747870

反応方程式

10-[4-(N-phenyl-2-benzimidazolyl)phenyl]phenothiazine

m-chloroperbenzoic acid

KOH

→

10-[4-(N-Phenyl-2-benzimidazolyl)phenyl]phenothiazine 5,5-dioxide

溶媒

methylene chloride

反応条件

後処理

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

実験手順

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.

出典