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(8-Phenyl-1,4-dioxaspiro[4.5]dec-8-yl)MethanaMine synthesis

2synthesis methods
4-Cyano-4-phenylcyclohexanone ethylene ketal

51509-98-9
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(8-Phenyl-1,4-dioxaspiro[4.5]dec-8-yl)MethanaMine

443687-93-2
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Yield:443687-93-2 90%

Reaction Conditions:

with lithium aluminium tetrahydride in tetrahydrofuran; for 2 h;Heating / reflux;

Steps:

1.3

Compound 3: To a solution of 2 (12.9 g, 50 mmol) in THF (100 mL) was added dropwise via cannula a 1.0 M solution of LAH in THF (60 ml, 60 mmol) The resulting solution was stirred at reflux for 2 hours then cooled to 0° C. and carefully quenched with 4N NaOH (4 mL). The mixture was filtered through a short pad of Na2SO4 and the filter cake washed with THF. Volatiles were removed in vacuo to provide 3 an oil (11.3 g, >90%), which was subjected to the following reaction without further purification.

References:

US2005/250783,2005,A1 Location in patent:Page/Page column 18