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HRID 2396633作成日:2026年10月26日

Sodium hydride → ethyl (E) 6-(4-methoxyethoxymethoxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2-(dimethylphosphono)-4-methyl-4-hexenoate

https://huagongshe.com/reaction/2396633

反応式

関与物質

役割名称HCID仕込み量
反応物Sodium hydrideHCID 24758—
反応物Ethyl (dimethoxyphosphinoyl)acetateHCID 67555—
反応物3-[6-(1,3-dihydro-6-methoxy-4-methoxyethoxymethoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2-(S),4-dimethylhexanoyl)-4-(R)-isopropyl-2-oxazolidinoneHCID 131719267—
溶媒DimethylformamideHCID 6228—
生成物ethyl (E) 6-(4-methoxyethoxymethoxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2-(dimethylphosphono)-4-methyl-4-hexenoateHCID 131719269—

反応手順

To a solution of ethyl dimethylphosphonoacetate (135 mg) in DMF (5 ml) at 0° was added 50% NaH/oil (33 mg), and the mixture stirred for 10 minutes. (E) 4-(1,3-dihydro-6-methoxy-4-methoxyethoxymethoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2-methylbut-2-enyl bromide (600 mg) was added at the same temperature and allowed to reach room temperature in 30 minutes. The reaction was poured onto water and extracted with EtOAc. The organic layers were washed with water, dried over sodium sulfate, and evaporated to give the crude product which was purified by flash chromatography (CH2Cl2 followed by BtOAc) to obtain ethyl (E) 6-(4-methoxyethoxymethoxy-1,3-dihydro-6-methoxy-7-methyl-3-oxoisobenzofuran-5-yl)-2-(dimethylphosphono)-4-methyl-4-hexenoate as an oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US05493030
出典データセットuspto-grants-1996_02
ORD IDord-577cc2ea46e5470dbabe81076943806d
出典メモuspto-grants-1996_02