반응 #480163

반응 방정식

intermediate 58

Methyl 6-(cyclohexylamino)-5-nitronicotinate

ethyl 4-hydroxybenzimidate hydrochloride

→

intermediate 59

수율 88.0%

Methyl 3-cyclohexyl-2-(4-hydroxyphenyl)-3H-imidazo[4,5-b]pyridine-6-carboxylate

수율 88.0%

용매

methanol

반응 조건

후처리

1. 1
   온도at reflux for 22 h
2. 2
   여과the precipitated solid was collected by vacuum filtration
3. 3
   세척washed sparingly with cold methanol

실험 절차

A solution of intermediate 58 (5.0 g, 20.0 mmol) and ethyl 4-hydroxybenzimidate hydrochloride (6.0 g, 30.0 mmol) in methanol (67 mL) was heated at reflux for 22 h. The reaction mixture was then cooled to rt and the precipitated solid was collected by vacuum filtration and washed sparingly with cold methanol to afford intermediate 59 as a white solid (6.13 g, 88%). ESI-MS m/e 352.2 (M+1).

출처