Reaktion #95965

Reaktionsgleichung

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

Lösungsmittel

diethyl ether

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

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.

Quelle