反应详情

温度

155 °C

5-amino-1-(2-chlorobenzyl)-1H-1,2,3-triazole-4-carboxamide (10.80 g, 42.9 mmol, Eq: 1.00) was suspended in N,N-dimethylacetamide (50.2 g, 54.0 ml). Pyridine (5.1 g, 5.19 ml, 64.4 mmol, Eq: 1.5) was added followed by pivaloyl chloride (7.84 g, 8.00 ml, 64.4 mmol, Eq: 1.5) and the reaction mixture was heated to ca 80° C. After 3 h reaction (and complete conversion of the starting material to the intermediate), KHCO3 (21.6 g, 215 mmol, Eq: 5.00) was added and the suspension was heated to Tj=155° C. for 24 h to convert the 1-[(2-chlorophenyl)methyl]-5-(2,2-dimethylpropanoylamino)triazole-4-carboxamide intermediate to the product. The reaction mixture was cooled to RT and water (254 g, 254 ml) was added dropwise over 30 min. The brown suspension was cooled to 0° C., stirred for 1 h30 min and was filtered. The filter cake was washed with water (43.2 g, 43.2 ml) and dried at 500° C./5 mbar to give 11 g of the title compound as an off-white powder. MS(m/e): 318.0 (MH+).

1. temperaturethe reaction mixture was heated to ca 80° C
2. additionwas added
3. temperatureThe reaction mixture was cooled to RT
4. temperatureThe brown suspension was cooled to 0° C.
5. filtrationwas filtered
6. washThe filter cake was washed with water (43.2 g, 43.2 ml)
7. customdried at 500° C./5 mbar