反应 #1747865

反应方程式

hydrochloric acid

benzoyl chloride

10-(2-hydroxyphenyl)phenothiazine

→

2-(Phenothiazin-10-yl)phenyl benzoate

溶剂

pyridine

反应条件

后处理

1. 1
   温度the reaction solution was heated to 60-65° C.
2. 2
   workup.STIRRINGstirred at this temperature for 15 min
3. 3
   温度After cooling to room temperature
4. 4
   workup.STIRRINGthe suspension was then stirred overnight
5. 5
   workup.STIRRINGstirred for 1 h
6. 6
   过滤The suspension was filtered through a glass frit
7. 7
   洗涤The residue was washed
8. 8
   其他dried at 60° C. under reduced pressure
9. 9
   其他were obtained

实验过程

16.0 g (114 mmol) of benzoyl chloride were added dropwise at 0-5° C. with stirring to a solution of 4.00 g (13.7 mmol) of 10-(2-hydroxyphenyl)phenothiazine in 24 ml of pyridine within 30 min. After stirring at room temperature for 2 h, the reaction solution was heated to 60-65° C. and stirred at this temperature for 15 min. After cooling to room temperature, the suspension was then stirred overnight. After adding 300 ml of ice-water, the suspension was admixed slowly with 19 ml of conc. hydrochloric acid (pH 0.9) and stirred for 1 h. The suspension was filtered through a glass frit. The residue was washed to neutrality with 2 l of water and dried at 60° C. under reduced pressure. 2.87 g (53% of theory) of colorless microcrystals having a melting point of 144-148° C. were obtained.

来源