반응 #1747865

반응 방정식

hydrochloric acid

benzoyl chloride

10-(2-hydroxyphenyl)phenothiazine

→

2-(Phenothiazin-10-yl)phenyl benzoate

용매

pyridine

반응 조건

후처리

1. 1
   온도the reaction solution was heated to 60-65° C.
2. 2
   workup.STIRRINGstirred at this temperature for 15 min
3. 3
   온도After cooling to room temperature
4. 4
   workup.STIRRINGthe suspension was then stirred overnight
5. 5
   workup.STIRRINGstirred for 1 h
6. 6
   여과The suspension was filtered through a glass frit
7. 7
   세척The residue was washed
8. 8
   기타dried at 60° C. under reduced pressure
9. 9
   기타were obtained

실험 절차

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.

출처