반응 #626971

반응 방정식

5-(6-chloroimidazo[2,1-f]pyridazin-2-yl)-2-methyl-aniline

acetonitrile

trimethylacetyl chloride

→

title compound

수율 94.0%

N-[5-(6-chloroimidazo[2,1-f]pyridazin-2-yl)-2-methyl-phenyl]-2,2-dimethyl-propanamide

수율 94.0%

용매

pyridine

반응 조건

후처리

1. 1
   농축The mixture is concentrated
2. 2
   세척washed once with HCl (20 mL, 1M)
3. 3
   기타Organic layer is dried
4. 4
   농축concentrated
5. 5
   기타purified on silica gel chromatography (0-100% EtOAc in Hexanes)

실험 절차

A 40 mL vial is charged with 5-(6-chloroimidazo[2,1-f]pyridazin-2-yl)-2-methyl-aniline (0.85 g, 3.28 mmol), acetonitrile (14 mL) and pyridine (0.450 mL). The mixture is added trimethylacetyl chloride (0.628 mL, 0.0051 mol) and stirred for 20 min at 80° C. The mixture is concentrated, taken up in EtOAc (35 mL) and washed once with HCl (20 mL, 1M) and then NaOH (20 mL, 1M). Organic layer is dried, concentrated and purified on silica gel chromatography (0-100% EtOAc in Hexanes) to give the title compound (1.05 g, 94% yield). LCMS m/z=343.5 [M+H]+, tR=2.39 min. (compound same as Example 118)

출처