3-CHLORO-6-IODO-4,5-DIMETHYLPYRIDAZINE synthesis

Yield:1032714-27-4 77%

Reaction Conditions:

Stage #1: 3,6-dichloro-4,5-dimethylpyridazinewith hydrogen iodide;sodium iodide in water at 120; for 0.166667 h;Microwave irradiation;
Stage #2: with water;sodium carbonate in water;

Steps:

10

Description 10; 3-Chloro-6-iodo-4,5-dimethyl-pyridazine (DlO); N - N A mixture of D9 (0.2 g, 1.13 mmol), sodium iodide (0.420 g, 2.8 mmol) and hydroiodic acid (57 wt.% in water, 2 ml) was stirred at 120 ⁰C for 10 min., under microwave irradiation. The mixture was then poured into an aqueous saturated solution of sodium carbonate, Na₂S₂O₃, water and dichloromethane. The organic phase was separated, filtered over cotton, and the solvent evaporated in vacuo. The residue was purified by column chromatography (dichloromethane / heptane 1 :1 to 8:2) to yield DlO (0.235 g, 77%) as a solid. C₆H₆CUN₂ requires 268; Found 269 (MH⁺).

References:

WO2008/68277,2008,A1 Location in patent:Page/Page column 21