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HRID 878417作成日:2026年10月26日

Dimethylamine → ethyl 4-(N,N-dimethylamidino)benzoate

https://huagongshe.com/reaction/878417

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylamineHCID 674—
反応物Ethyl 4-cyanobenzoateHCID 81589—
反応物Sodium BicarbonateHCID 516892—
反応物HCID 178506865HCID 178506865—
溶媒TetrahydrofuranHCID 8028—
溶媒HexaneHCID 8058—
生成物ethyl 4-(N,N-dimethylamidino)benzoateHCID 22631319—

反応手順

To a tetrahydrofuran solution of 2M dimethylamine, 2.3M hexane solution of hexyllithium was slowly added over a period of at least three (3) hours while maintaining the temperature at between −8° C. and −12° C. This solution was added to the tetrahydrofuran solution of ethyl-4-cyanobenzoate (F) while maintaining the temperature between −8° C. and −12° C. The completion of the reaction was confirmed by HPLC, and the solution temperature was adjusted to between −8° C. and 3° C. The reaction mixture was slowly added to the cold solution of aqueous sodium bicarbonate solution and the desired ethyl-4-(N,N-dimethylcarbamimidoyl)benzoate (G) was extracted with ethyl acetate. The ethyl acetate layer was dried, filtered and evaporated under vacuum to afford ethyl-4-(N,N-dimethylcarbamimidoyl)benzoate (G) as a white solid.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08987463B2
出典データセットuspto-grants-2015_03
ORD IDord-6b8c5798f8b844fb8f5d4e50764ea7c2
出典メモuspto-grants-2015_03