反应详情

A reaction mixture comprising 3.0 g (0.01 mole) of 4-(5-tert-butyl-1,3,4-thiadiazol-2-ylcarbamoylmethyl)-2-aminothiazole, 50 ml of pyridine and 0.8 g (0.014 mole) of methyl isocyanate was heated at 35°-37° for four hours. The reaction solution was allowed to stand over the weekend at ambient temperature. Most of the pyridine was removed by employing a rotary evaporator. The residue was mixed with hexane and the crude solid was collected. The filter cake was well washed with ethyl acetate. There was obtained 2.5 g of product, m.p. 190° (dec.). N.M.R. (dimethyl-d6 sulfoxide) ∂ 1.4 [C(CH3)3 ], 2.6 (CH3, doublet), 3.7 (CH2), 6.7 (hetero-aromatic).

1. customto stand over the weekend at ambient temperature
2. customMost of the pyridine was removed
3. customa rotary evaporator
4. additionThe residue was mixed with hexane
5. customthe crude solid was collected
6. washThe filter cake was well washed with ethyl acetate