반응 #76208

반응 방정식

Rochelle salt

methyl 4-(4-chlorophenyl)-2-(2-methylimidazol-1-yl)-5-oxazolepropionate

sodium bis(2-methoxyethoxy)aluminum hydride

→

title compound

수율 77.3%

4-(4-Chlorophenyl)-5-(3-hydroxypropyl)-2-(2-methylimidazol-1-yl)oxazole

수율 77.3%

용매

toluene

반응 조건

후처리

1. 1
   여과the precipitated crystals were collected by filtration
2. 2
   세척The obtained crystals were washed with 10% Rochelle salt and water
3. 3
   기타dried under reduced pressure
4. 4
   workup.ADDITIONThe residue was suspended in a mixture of ethyl acetate (717 mL) and isopropyl ether (2866 mL)
5. 5
   여과The obtained crystals were collected by filtration

실험 절차

To a solution of methyl 4-(4-chlorophenyl)-2-(2-methylimidazol-1-yl)-5-oxazolepropionate (716.6 g) in toluene (7166 ml) was added dropwise sodium bis(2-methoxyethoxy)aluminum hydride (70% toluene solution, 957.6 g) at not higher than 5° C. over 4 h. To the reaction mixture was added dropwise 10% aqueous Rochelle salt solution (7166 ml) at not higher than 10° C. and the precipitated crystals were collected by filtration. The obtained crystals were washed with 10% Rochelle salt and water, and dried under reduced pressure. The residue was suspended in a mixture of ethyl acetate (717 mL) and isopropyl ether (2866 mL) and the suspension was stirred at room temperature for 3 h. The obtained crystals were collected by filtration to give the title compound (509 g, yield: 77.3%).

출처