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1,2-Cyclobutanedione synthesis

8synthesis methods
-

Yield:33689-28-0 96.7%

Reaction Conditions:

in ethyl acetate;

Steps:

5.a Production of 3-hydroxy-2-cyclobuten-1-one dicyclohexylammonium salt

(a) A solution of 7.1 g of dicyclohexylamine (98 percent; 38.3 mmol) in 15 ml of ethyl acetate was instilled in a suspension of 3.0 g of 1,3-cyclobutanedione (97 percent; 34.6 mmol) in ethyl acetate (52.2 ml) at 20° C. in 15 minutes. After 1 hour of stirring at room temperature, the suspension was washed four times with ethyl acetate and dried under vacuum. 9.4 g of the title product with a content of 94.7 percent (according to HPLC), corresponding to a yield of 96.7 percent, relative to cyclobutanedione, was obtained. Data for the title compound was: Melting point: 188° C-188.7° C.

References:

US5118847,1992,A

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