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HRID 351492作成日:2026年10月27日

Triethylamine → 1,3-Dioxan-5-yl 5-norbornene-2-carboxylate

https://huagongshe.com/reaction/351492

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物1,3-Dioxolane-4-methanolHCID 21618—
反応物Bicyclo(2.2.1)hept-5-ene-2-carbonyl chlorideHCID 98233—
反応物(1,3-Dioxolan-4-yl)methyl 5-norbornene-2-carboxylateHCID 22713062—
溶媒WaterHCID 962—
溶媒TolueneHCID 1140—
生成物1,3-Dioxan-5-yl 5-norbornene-2-carboxylateHCID 6991020095%

反応手順

To a mixture of 104 g of glycerol formal, 111 g of triethylamine and 300 ml of toluene, 157 g of 5-norbornene-2-carbonyl chloride was added over one hour at 20° C. After 5 hours of stirring, 200 ml of water was added to stop the reaction and the mixture was allowed to separate. The organic layer was washed with water and saturated sodium chloride water, dried over anhydrous sodium sulfate, and concentrated in vacuum. It was further purified by vacuum distillation, obtaining 213 g of a mixture of (1,3-dioxolan-4-yl)methyl 5-norbornene-2-carboxylate and 1,3-dioxan-5-yl 5-norbornene-2-carboxylate (boiling point 111-115° C./530 Pa, yield 95%).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06743566B2
出典データセットuspto-grants-2004_06
ORD IDord-58449c2172d64bb194918c6cc2617234
出典メモuspto-grants-2004_06