반응 #1573923

반응 방정식

NaOH

N-(3-[1,3]dioxolan-2-yl-phenyl)-5-methyl-nicotinamide

HCl

Water

→

crude title compound

N-(3-Formyl-phenyl)-5-methyl-nicotinamide

용매

dioxane

1,4-dioxane

반응 조건

후처리

1. 1
   기타to get pH 10
2. 2
   추출The mixture is extracted twice with EtOAc (100 mL)
3. 3
   건조The combined organic phases are dried over MgSO4
4. 4
   여과filtered
5. 5
   기타evaporated

실험 절차

A solution of N-(3-[1,3]dioxolan-2-yl-phenyl)-5-methyl-nicotinamide (3.0 g, 10.55 mmol) in dioxane (50 mL) is treated with a 4M HCl in 1,4-dioxane (30 mL). The mixture is heated at 60° C. for 3 h. Water (100 mL) is added to the mixture followed by NaOH 2M (70 mL) solution to get pH 10. The mixture is extracted twice with EtOAc (100 mL). The combined organic phases are dried over MgSO4, filtered and evaporated. The crude title compound is obtained as a brownish solid (1.744 g. 69%) LC-MS A: tR=0.58 min; [M+H]+=241.24.

출처