반응 #56274

반응 방정식

urea

5-amino-3-trichloromethyl-1,2,4-thiadiazole

phenyl isocyanate

benzene

→

pure product

수율 24.0%

1,3-Diphenyl-5-(3-Trichloromethyl-1,2,4-thiadiazol-5-yl)biuret

수율 24.0%

용매

methanol

반응 조건

후처리

1. 1
   workup.ADDITIONA magnetic stirring bar was added
2. 2
   기타the vessel sealed
3. 3
   기타The stirred reaction mixture
4. 4
   기타precipitates
5. 5
   기타The by-product was removed by filtration
6. 6
   농축the filtrate concentrated in vacuo
7. 7
   기타to leave 9.0 grams of crude product

실험 절차

A glass pressure vessel was charged with 5.5 grams (0.03 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole, 7.4 grams (0.06 mole) phenyl isocyanate and 50 milliliters benzene. A magnetic stirring bar was added and the vessel sealed. The stirred reaction mixture was heated at 145° C. for 1.5 hours and then allowed to cool to room temperature where a urea by-product precipitates. The by-product was removed by filtration and the filtrate concentrated in vacuo to leave 9.0 grams of crude product. Trituration with cold methanol gave 2.8 grams (24% yield) of pure product; m.p. 170° C.

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