반응 #95965

반응 방정식

water

sodium hydroxide

water

lithium aluminum hydride

8-cyano-[1,4-dioxaspiro[4.5]dec-8-yl]dimethylamine

→

8-(dimethylamino)-1,4-dioxaspiro[4.5]decane-8-methanamine

용매

diethyl ether

반응 조건

후처리

1. 1
   workup.ADDITION4,065,573, Example 41, part B) was added over 20 minutes
2. 2
   여과The inorganic gel in the mixture was filtered off
3. 3
   기타The filtrate was dried by evaporation under vacuum

실험 절차

A 0.4 g portion of lithium aluminum hydride (LAH) is cooled in 10 ml of diethyl ether under nitrogen atmosphere. Then 2.0 g of 8-cyano-[1,4-dioxaspiro[4.5]dec-8-yl]dimethylamine (U.S. Pat. No. 4,065,573, Example 41, part B) was added over 20 minutes while stirring at room temperature. Then, in turn, there was added 0.4 ml of water, 0.4 ml of 15 percent sodium hydroxide and 1.2 ml of water. The inorganic gel in the mixture was filtered off. The filtrate was dried by evaporation under vacuum. A thin layer chromatography (tlc) sample analysis showed the residue to be largely one spot material. The Nuclear Magnetic Resonance spectrum (NMR) for this material was very good for the above-named chemical intermediate.

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