반응 #92939

반응 방정식

2,6-difluorobenzoylisocyanate

4-(α-cyclopropyl-4-chlorobenzylideneaminooxymethyl)aniline

→

desired product

N-(2,6-difluorobenzoyl)-N'-[4-(α-cyclopropyl-4-chlorobenzylideneaminooxymethyl)phenyl]urea

용매

diethyl ether

diethylether

반응 조건

후처리

1. 1
   온도with external cooling at 0°-10° C
2. 2
   세척washed with diethyl ether
3. 3
   기타dried
4. 4
   기타The product obtained in a yield of 76.0 g
5. 5
   기타was chromatographed over silica, chloroform being

실험 절차

36.6 g of 2,6-difluorobenzoylisocyanate in 50 ml of dry diethyl ether were added to a solution of 59.0 g 4-(α-cyclopropyl-4-chlorobenzylideneaminooxymethyl)aniline in 700 ml of dry diethylether with external cooling at 0°-10° C. After stirring for 3 hours at 0°-10° C. the formed precipitate was sucked off, washed with diethyl ether, and dried. The product obtained in a yield of 76.0 g was chromatographed over silica, chloroform being used as an eluent. The desired product was isolated in a yield of 60,7 g having a purity of at least 95% (PMR). The product obtained had a melting range of 145°-175° C. and comprised the syn- and anti-form in approximately equal amounts. In another experiment the desired product was obtained as a mixture of the syn- and anti-form in a ratio of 85:15; melting point 187°-191° C.

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