반응 #327991

반응 방정식

1,4-Phenylene diisocyanate

triethylamine

1-methoxy-4-trifluoropropynylbenzene

4-nitrobutanoic acid methyl ester

→

trifluoromethyl isoxazole

수율 56.5%

용매

toluene

반응 조건

후처리

1. 1
   여과The reaction solution was filtered with celite
2. 2
   workup.DISTILLATIONthe solvent was then distilled away
3. 3
   기타The residue was purified by silica gel column chromatography (hexane/ethyl acetate)

실험 절차

1,4-Phenylene diisocyanate (597.1 mg, 3.73 mol) and triethylamine (780 μL, 5.60 mmol) were added to a solution of 1-methoxy-4-trifluoropropynylbenzene (373.2 mg, 1.86 mmol) and 4-nitrobutanoic acid methyl ester (441.5 mg, 2.80 mmol) in toluene (10 mL). Using a microwave reactor, the obtained mixture was stirred at 150° C. for 2 hours. The reaction solution was filtered with celite, and the solvent was then distilled away. The residue was purified by silica gel column chromatography (hexane/ethyl acetate) to obtain a trifluoromethyl isoxazole compound (144.0 mg, yield: 25%).

출처