반응 #4746

반응 방정식

3-((methylpiperidin-1-yl)methyl) phenol

sodium hydride

DMF

Na2SO4

LiAlH4

4chlorobutyronitrile

→

4-[3-[(3-Methylpiperidin-1-yl)methyl]phenoxy]butanamine

용매

ether

H2O

반응 조건

후처리

1. 1
   workup.STIRRINGthe reaction mixture is stirred at 60° C. for 7 hours
2. 2
   추출extracted with ether
3. 3
   세척the organic phase is washed with 5% NaOH
4. 4
   기타After removal of the inorganic constituents
5. 5
   여과by filtration and evaporation of the solvent under vacuum, 3.66 g of a pale yellow oil
6. 6
   workup.WAITare left behind

실험 절차

5.13 g (0.025 mol) of 3-((methylpiperidin-1-yl)methyl) phenol (Example 64 a) are added to a suspension of 1.0 g (0.025 mol) of sodium hydride (60%) in absolute DMF and the mixture is stirred overnight at room temperature. After the addition of 2.58 g (0.025 mol) of 4chlorobutyronitrile, the reaction mixture is stirred at 60° C. for 7 hours, and then poured into ice water and extracted with ether, and the organic phase is washed with 5% NaOH. After dehydration over Na2SO4, the ethereal phase is introduced dropwise into a suspension of 1.14 g (0.03 mol) of LiAlH4 in absolute ether and then hydrolysed with 2.2 ml H2O. After removal of the inorganic constituents by filtration and evaporation of the solvent under vacuum, 3.66 g of a pale yellow oil are left behind.

출처