반응 #55283

반응 방정식

3-carbethoxythiomorpholine

4-chloro-2-fluorophenylisocyanate

→

3-carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine

수율 87.7%

용매

n-hexane

ether

반응 조건

후처리

1. 1
   기타A heavy oil formed
2. 2
   workup.ADDITIONafter the addition
3. 3
   기타The oil crystallized
4. 4
   workup.STIRRINGafter stirring at room temperature for 15 min
5. 5
   여과The precipitate was collected by filtration

실험 절차

An emulsion of 14 g of 3-carbethoxythiomorpholine in 50 ml of n-hexane was added dropwise to a solution of 14 g of 4-chloro-2-fluorophenylisocyanate in 60 ml of anhydrous ether at 15° to 28° C. with stirring. A heavy oil formed after the addition. The oil crystallized after stirring at room temperature for 15 min. The precipitate was collected by filtration to give 24.3 g of 3-carbethoxy-4-(4-chloro-2-fluorophenylaminocarbonyl)thiomorpholine, m.p. 111.5°-112.5° C.

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