2-Benzyloctahydro-1H-pyrido[1,2-a]pyrazine synthesis
- Product Name:2-Benzyloctahydro-1H-pyrido[1,2-a]pyrazine
- CAS Number:36067-99-9
- Molecular formula:C15H22N2
- Molecular Weight:230.35
![2-Benzylhexahydro-6H-pyrido[1,2-a]pyrazine-1,4-dione](/CAS/20180703/GIF/1049651-57-1.gif)
1049651-57-1
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Yield:36067-99-9 70%
Reaction Conditions:
Stage #1: 2-benzyl-hexahydro-6H-pyrido[1,2-a]pyrazine-1,4-dionewith lithium aluminium tetrahydride in tetrahydrofuran at 0; for 3 h;Heating / reflux;
Stage #2: with sodium hydroxide in water;
Steps:
F.4
4. Synthesis of 2-benzyl-octahydro-1H-pyrido[1,2-a]pyrazine Into a 5000 mL 3-necked round-bottom flask was placed a solution of 2-benzyl-hexahydro-6H-pyrido[1,2-a]pyrazine-1,4-dione (96 g, 353.05 mmol) in THF (2000 mL) while cooling to 0° C. To the above was added LiAlH (91.67 g, 2.42 mol) in several batches. The resulting solution was allowed to react with stirring, for 3 hours while the temperature was maintained at reflux in a bath of oil. The reaction progress was monitored by TLC(CH2Cl2MeOH=10:1). The mixture was added 92 mL H2O, 276 mL NaOH solution and 92 mL H2O. A filtration was performed. The mixture was dried over MgSO4 and concentrated by evaporation under vacuum using a rotary evaporator. The residue was purified by eluding through a column with a 1:1 ethyl acetate/petroleum ether solvent system. This resulted in 60 g (70%) of 2-benzyl-octahydro-1H-pyrido[1,2-a]pyrazine as a yellow solid.
References:
US2008/200471,2008,A1 Location in patent:Page/Page column 38-39; 39
157634-02-1
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