反応 #56274

反応方程式

urea

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

phenyl isocyanate

benzene

→

pure product

収率 24.0%

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

収率 24.0%

溶媒

methanol

反応条件

後処理

1. 1
   workup.ADDITIONA magnetic stirring bar was added
2. 2
   その他the vessel sealed
3. 3
   その他The stirred reaction mixture
4. 4
   その他precipitates
5. 5
   その他The by-product was removed by filtration
6. 6
   濃縮the filtrate concentrated in vacuo
7. 7
   その他to leave 9.0 grams of crude product

実験手順

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.

出典