1H-Pyrazole-3-carboxamide,1,5-dimethyl-(9CI) synthesis

Yield:54384-74-6 81%

Reaction Conditions:

Stage #1: 1,5-dimethyl-1H-pyrazole-3-carboxylic acidwith dichlorosulfoxide for 2 h;Reflux;
Stage #2: with ammonia in lithium hydroxide monohydrate at 0;

Steps:

III-57.1

A mixture of l-dimethyl-lH-pyrazole-S-carboxylic acid (10 g, 71.43 mmol) and SOCl₂ (25.5 g, 214.29 mmol) was refluxed for 2 hr. The mixture was concentrated under vacuum. The residue was added with 200 mL of NH₃-H₂O dropwise with stirring at 0 °C. The solids were collected by filtration, resulted in 8 g (81%) of l,5-dimethyl-lH-pyrazole-3- carboxamide as a white solid.

References:

WO2009/139834,2009,A1 Location in patent:Page/Page column 128-129