반응 #1063404

반응 방정식

phenol

2-isocyanato-4-methoxy-6-trifluoromethylpyrimidine

→

title compound

수율 87.0%

4-Methoxy-2-[(phenoxycarbonyl)amino]-6-trifluoromethylpyrimidine

수율 87.0%

용매

methylene chloride

반응 조건

후처리

1. 1
   workup.DISTILLATIONthe methylene chloride was distilled off under reduced pressure
2. 2
   workup.STIRRINGthe residue was stirred vigorously with 100 ml of a diisopropyl ether/hexane mixture (v/v 1:20), whereupon crystallization
3. 3
   여과The product was filtered off with suction
4. 4
   건조dried under reduced pressure from a water pump at 50° C

실험 절차

4.2 g of phenol (45 mmol) were added at 25° C. to a solution of 9.9 g of 2-isocyanato-4-methoxy-6-trifluoromethylpyrimidine (45 mmol) in 50 ml of methylene chloride. Stirring was carried out for 16 hours at 25° C., the methylene chloride was distilled off under reduced pressure and the residue was stirred vigorously with 100 ml of a diisopropyl ether/hexane mixture (v/v 1:20), whereupon crystallization occurred. The product was filtered off with suction and dried under reduced pressure from a water pump at 50° C. The title compound (12.2 g; 87% of theory) was obtained as colorless crystals of melting point 85°-88° C.

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