2-methyl-2,7-diazaspiro[4.5]decane(SALTDATA: FREE) synthesis
- Product Name:2-methyl-2,7-diazaspiro[4.5]decane(SALTDATA: FREE)
- CAS Number:1086395-66-5
- Molecular formula:C9H18N2
- Molecular Weight:154.25
![2,7-Diazaspiro[4.5]decan-1-one,2-Methyl-, (Hydrochloride) (1:1)](/CAS/20180808/GIF/1153767-88-4.gif)
1153767-88-4
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Yield:1086395-66-5 60%
Reaction Conditions:
Stage #1: 2-methyl-2,7-diazaspiro[4.5]decan-1-one hydrochloridewith lithium aluminium tetrahydride in tetrahydrofuran at 20 - 60; for 2 h;
Stage #2: with sodium hydroxide in tetrahydrofuran;water;
Steps:
5; 6
LiAlH4 (80 mg, 2.1 mmol) was added as a solid (exothermic and foaming occurred) to a slurry of 2-methyl-2,7-diazaspiro[4.5]decan-1-one, HCl (160 mg, 0.78 mmol) in THF (3 mL) and the reaction was stirred 1 h at rt, and then 1 h at 60° C. The reaction mixture was cooled to rt and then slowly quenched with H2O (3 mL) and 1M NaOH (0.5 mL) and stirred ON. The resulting emulsion was diluted with DCM (20 mL) and filtered through celite (flushing with DCM) and the layers were separated. The organic layers was dried (MgSO4), filtered and concentrated to yield 2-methyl-2,7-diazaspiro[4.5]decane (70 mg. 0.45 mmol, 60%) as a clear colorless oil, which was used without further purification.
References:
US2009/130056,2009,A1 Location in patent:Page/Page column 44-45
6283-71-2
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1433194-42-3
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1086395-66-5
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$45.00/25mg