반응 #161356

반응 방정식

4-fluoro-N-(2-hydroxyphenyl)-3-nitrobenzanilide

p-toluenesulfonic acid monohydrate

→

title compound

수율 70.0%

2-(4-fluoro-3-nitrophenyl)benzoxazole

수율 70.0%

용매

toluene

반응 조건

후처리

1. 1
   온도heated
2. 2
   온도to reflux for 4 hours
3. 3
   workup.DISTILLATIONafter the solvent was distilled off
4. 4
   workup.ADDITIONsaturated aqueous sodium hydrogen carbonate solution was added
5. 5
   workup.STIRRINGthis was stirred for 10 minutes at room temperature
6. 6
   여과The precipitated crystals were filtered off
7. 7
   세척after washing with toluene the crystals
8. 8
   기타were dried

실험 절차

To a suspension of 4-fluoro-N-(2-hydroxyphenyl)-3-nitrobenzanilide (see Working Example 15-1) (2.00 g, 7.24 mmol) in toluene (50 mL) was added p-toluenesulfonic acid monohydrate (2.07 g, 10.9 mmol), and this was stirred and heated to reflux for 4 hours. After the reaction was complete, this was cooled to room temperature, and after the solvent was distilled off, saturated aqueous sodium hydrogen carbonate solution was added and this was stirred for 10 minutes at room temperature. The precipitated crystals were filtered off, and after washing with toluene the crystals were dried to yield the title compound (1.30 g, 70% yield) as yellow crystals.

출처