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HRID 461465作成日:2026年10月26日

Dimethylformamide → N-(N-[Bicyclo[2.2.1]hept-2-en-5-ylmethyl]carbamoyl)-2-phenylethenesulfonamide

https://huagongshe.com/reaction/461465

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylformamideHCID 6228—
反応物Sodium hydrideHCID 24758—
反応物2-PhenylethenesulfonamideHCID 257501—
反応物N'-(bicyclo[2.2.1]hept-5-en-2-ylmethyl)-N,N-diphenylureaHCID 12282081—
溶媒Diethyl EtherHCID 3283—
生成物N-(N-[Bicyclo[2.2.1]hept-2-en-5-ylmethyl]carbamoyl)-2-phenylethenesulfonamideHCID 54231290—

反応手順

To a solution of 1.8 g. of 2-phenylethenesulfonamide and 4.8 g. of 1,1-diphenyl-3-(bicyclo[2.2.1]hept-2-en-5-ylmethyl)urea in 20 ml. of N,N-dimethylformamide, is added, with stirring 0.64 g. of a 56.6% dispersion of sodium hydride in mineral oil. The mixture is stirred at ambient temperature overnight, during which time a heavy precipitate forms. To the reaction mixture is then added 200 ml. of ether. After stirring for 15 minutes, the precipitate is filtered off. It is dissolved in 50 ml. of water, and then the crude product is precipitated by acidification usng concentrated hydrochloric acid. It is filtered off and recrystallized from aqueous acetone. The yield is 1.9 g. (56%) of a solid, m.p. 161°-163.5° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04062960
出典データセットuspto-grants-1977_12
ORD IDord-0f04b68366f946ca8929ad0918755bef
出典メモuspto-grants-1977_12