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1,2-dioxo-1,2-dihydroacenaphthylene-5-carbonitrile synthesis

4synthesis methods
773837-37-9 Synthesis
sodium:cyanide

773837-37-9
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26254-35-3 Synthesis
5-bromoacenaphthylene-1,2-dione

26254-35-3
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1,2-dioxo-1,2-dihydroacenaphthylene-5-carbonitrile

109179-38-6
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Yield:109179-38-6 11 g

Reaction Conditions:

with bis(tri-t-butylphosphine)palladium(0) in tetrahydrofuran;acetonitrile; for 1 h;

Steps:

5 Synthesis of Compound 4-55c

The compound D (15 g, 57.5 mmol) and NaCN (1.1 eq., 3.1 g) were added to acetonitrile and THF solvent and the mixture was heated to 70 ° C. The catalyst was prepared by dissolving bis(tri-tert-butylphosphine)palladium (0.01 eq. And the reaction was continued for about 1 hour. After completion of the reaction, the reaction mixture was cooled to room temperature, and the solid was immediately filtered. The obtained solid was dissolved in dichloromethane, charcoal was added thereto, and the mixture was stirred for about 2 hours to filter with celite / silica. The solvent was evaporated to give compound 4-55c (11 g, 52.9 mmol).

References:

KR2017/65974,2017,A Location in patent:Paragraph 0269; 0270; 0275; 0276