반응 #93374

반응 방정식

alpha-isopropyl-alpha-[3-[N-[3-(3-hydroxymethylphenoxy)propyl]amino]propyl]-3,4,5-trimethoxyphenyl acetonitrile

formalin

sodium borohydride

→

desired compound

수율 25.7%

Alpha-isopropyl-alpha-[3-[N-[3-(3-hydroxymethylphenoxy)propyl]-N-methylamino]propyl]-3,4,5-trimethoxyphenylacetonitrile

수율 25.7%

용매

methanol

반응 조건

후처리

1. 1
   온도After cooling, to the solution
2. 2
   기타The solvent was removed and to the residue
3. 3
   workup.ADDITIONwas added water
4. 4
   추출The solution was extracted with chloroform
5. 5
   세척the extract was washed with water
6. 6
   기타dried
7. 7
   기타evaporated
8. 8
   기타The residue was chromatographed on silica gel using 10% methanol-chloroform as an eluent

실험 절차

A solution of 2.80 g of alpha-isopropyl-alpha-[3-[N-[3-(3-hydroxymethylphenoxy)propyl]amino]propyl]-3,4,5-trimethoxyphenyl acetonitrile and 4.84 g of 37% formalin in 70 ml of methanol was refluxed for 1 hour. After cooling, to the solution was added 2.25 g of sodium borohydride and the solution was stirred for 1 hour at room temperature. The solvent was removed and to the residue was added water. The solution was extracted with chloroform and the extract was washed with water, dried, and evaporated. The residue was chromatographed on silica gel using 10% methanol-chloroform as an eluent to give 0.74 g of the desired compound as a yellow oil.

출처