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HRID 235717作成日:2026年10月27日

Dimethylformamide → 3-(4-Tetradecylphenoxy)-1,2-propanediol

https://huagongshe.com/reaction/235717

反応式

関与物質

役割名称HCID仕込み量
反応物DimethylformamideHCID 6228—
反応物1,3-DioxolaneHCID 12586—
反応物Sodium hydrideHCID 24758—
反応物TetradecylphenolHCID 116800—
溶媒Diethyl EtherHCID 3283—
溶媒HexaneHCID 8058—
生成物3-(4-Tetradecylphenoxy)-1,2-propanediolHCID 20219899—

反応条件

温度80 °C

反応手順

An about 43.5 g portion of 4-tetradecyl phenol was added in portions to a suspension of about 10.8 g of prewashed sodium hydride in dimethylformamide. The mixture was refluxed about 11/2 hours, allowed to cool and about 37.8 g of 2,2-dimethyl-4-[[methylsulfonyl)oxy]methyl]-1,3-dioxolane was added. This mixture was heated to about 80° C. for about 24 hours; diluted with hexane and ether, washed with water and brine and evaporated. The residue was heated on a steam bath with about 500 ml of methanol and about 80 ml of dilute hydrochloric acid for one hour, cooled, partially evaporated, the solid collected and recrystallized from methanol, giving about 38 g of the desired title compound, mp 81.5°-83.5° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04640913
出典データセットuspto-grants-1987_02
ORD IDord-65c54c27b3da49ca840c4785aa94538a
出典メモuspto-grants-1987_02