Реакция #56273

Уравнение реакции

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

methyl isocyanate

benzene

urea

→

product

Выход 65.0%

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

Выход 65.0%

Условия реакции

Обработка

1. 1
   workup.ADDITIONA magnetic stirring bar was added
2. 2
   Другоеthe vessel sealed
3. 3
   ДругоеThe stirred reaction mixture
4. 4
   Другоеprecipitates
5. 5
   ДругоеThe by-product was removed by filtration
6. 6
   Концентрированиеthe filtrate concentrated in vacuo

Методика

A glass pressure vessel was charged with 27.5 grams (0.13 mole) 5-amino-3-trichloromethyl-1,2,4-thiadiazole, 17.9 grams (0.31 mole) methyl isocyanate, and 250 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 27.2 grams (65% yield) of product. Recrystallization from methanol gave an analytically pure sample; m.p. 94° C.

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