Hydrochloric Acid → 7-oxa-1,3-diazaspiro[4.4]nonane-2,4-dione

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Reaction Steps

A solution of 19.2 g of ammonium carbonate in 42 ml of ethanol and 28 ml of water is added to 10.0 g of 3-ketotetrahydrofuran. The resulting mixture is heated to 55° and to it is then added, dropwise, a solution of 6.3 g of potassium cyanide in 15 ml of water. The reaction mixture is stirred at 55° for 18 hrs. Thereafter the reaction mixture is evaporated in vacuo to dryness to obtain a residue. The residue is dissolved in a minimum of water and the mixture made acidic with 2 N hydrochloric acid. The first crop of the title product precipitates out on cooling and is filtered off. A second crop of the title product is obtained by concentrating the filtrate and cooling. The two combined crops are recrystalized from ethanol to give refined title product, m.p. 202°-204°.

Provenance & Evidence