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HRID 466214作成日:2026年10月26日

Pyridine → 1-Chlorocarbonyloxy-2,4-dimethoxynaphthalene

https://huagongshe.com/reaction/466214

反応式

関与物質

役割名称HCID仕込み量
反応物PyridineHCID 1049—
反応物PhosgeneHCID 6371—
反応物1-Hydroxy-2,4-dimethoxynaphthaleneHCID 12563547—
溶媒BenzeneHCID 241—
溶媒TetrahydrofuranHCID 8028—
生成物1-Chlorocarbonyloxy-2,4-dimethoxynaphthaleneHCID 19872730—

反応条件

温度25 °C

反応手順

To a solution of 1.27 g of 1-hydroxy-2,4-dimethoxynaphthalene, prepared as shown in Preparations 7 and 8, in 50 ml of tetrahydrofuran and 1 ml of pyridine is added 10 ml of a solution of 12.5% phosgene in benzene. The mixture is stirred overnight at 25° C., filtered and the filtrate evaporated under vacuum to afford crude 1-chlorocarbonyloxy-2,4-dimethoxynaphthalene. This chloroformate is dissolved in 50 ml of dry tetrahydrofuran and a solution of 1.14 g of diethylamine in 10 ml of tetrahydrofuran added. After 4 hours at room temperature the reaction mixture is diluted with ethyl acetate and washed with dilute hydrochloric acid. The organic phase is dried over sodium sulfate and solvent removed under reduced pressure to yield 1-diethylcarbamoyloxy-2,4-dimethoxynaphthalene.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05155132
出典データセットuspto-grants-1992_10
ORD IDord-ae719fbd2b7941a5bd62c52095c67ff3
出典メモuspto-grants-1992_10