Yield:1533443-11-6 94%

Reaction Conditions:

with N-iodo-succinimide in acetonitrile at 80; for 16 h;

Steps:

1 Compound 59.1. 5-Iodo-3,4-dimethyl-lH-pyrazole

Compound 59.1. 5-Iodo-3,4-dimethyl-lH-pyrazole. NIS (5.62g, 24.9mmol) was added portion-wise to a solution of 3,4-dimethyl-lH-pyrazole (2.0 g, 20.8 mmol) in CH₃CN (50 raL). The mixture was heated at 80 °C for 16 hours, upon where thick off-white solids formed. The mixture was cooled to room temperature and the solid were filtered, washed with cold CH₃CN and dried under reduced pressure to yiel 4.32g (94%) of the title compound as an off-white solid, m/z (ES+) 223 (M+H)⁺.

References:

WO2014/8197,2014,A1 Location in patent:Page/Page column 127