Reaktion #545337

Reaktionsgleichung

3-benzyl-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one

2-chlorocyclohexane

triethylamine

ethanol

→

rac-3-benzyl-8-(2-oxo-cyclohexyl)-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one

Reaktionsbedingungen

Aufarbeitung

1. 1
   Einengenconcentrated
2. 2
   Sonstigequenched with saturated NaHCO3
3. 3
   Extraktionextracted with ethyl acetate
4. 4
   WaschenThe combined organic extracts were washed with brine
5. 5
   Trocknendried over MgSO4
6. 6
   Filtrationfiltered
7. 7
   Sonstigeevaporated
8. 8
   SonstigePurification of the crude product over a silica gel plug (10:1) with n-heptane/AcOEt as eluent

Vorschrift

A solution of 0.30 g (0.93 mmol) 3-benzyl-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one, 0.14 g (1.0 mmol) 2-chlorocyclohexane, and 0.2 ml (1.4 mmol) triethylamine in ethanol was refluxed overnight. The reaction mixture was cooled to ambient temperature, concentrated and then quenched with saturated NaHCO3 and extracted with ethyl acetate. The combined organic extracts were washed with brine, dried over MgSO4, filtered and evaporated. Purification of the crude product over a silica gel plug (10:1) with n-heptane/AcOEt as eluent provided 0.14 g rac-3-benzyl-8-(2-oxo-cyclohexyl)-1-phenyl-1,3,8-triaza-spiro[4.5]decan-4-one as a light yellow oil; MS (ISP): 418.4 MH+.

Quelle