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HRID 16339作成日:2026年10月25日

Acetaldehyde → 2,6-Difluoro-alpha-methyl-3-pyridinemethanol

https://huagongshe.com/reaction/16339

反応式

関与物質

役割名称HCID仕込み量
反応物AcetaldehydeHCID 177—
反応物Hydrochloric AcidHCID 313—
反応物DiisopropylamineHCID 7912—
反応物2,6-DifluoropyridineHCID 73934—
反応物HCID 178418244HCID 178418244—
溶媒TolueneHCID 1140—
溶媒TetrahydrofuranHCID 8028—
溶媒Ethyl AcetateHCID 8857—
生成物2,6-Difluoro-alpha-methyl-3-pyridinemethanolHCID 22038305—

反応条件

温度-60 °C

反応手順

In nitrogen atmosphere, diisopropylamine (134 mL) was dropwise added to a solution mixture of an n-butyl lithium hexane solution (2.62 M, 368 mL) and tetrahydrofuran (800 mL) at −60° C. or below. The resulting reaction solution was stirred at −60° C. for 30 min, and then a tetrahydrofuran solution (100 mL) of 2,6-difluoropyridine (100 g) was dropwise added thereto at −60° C. or below. The resulting reaction solution was stirred at the same temperature for 1 hr, and then acetoaldehyde (97.6 mL) was dropwise added thereto. Then, a 2 N hydrochloric acid aqueous solution (1000 mL) was dropwise added to the reaction solution, and further ethyl acetate (1000 mL) and toluene (1000 mL) were added thereto. The organic layer was separated and concentrated under reduced pressure to give 129 g of the title compound. The physical property values of this compound were as follows:

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US07737141B2
出典データセットuspto-grants-2010_06
ORD IDord-491984727908469bba1e13abad271722
出典メモuspto-grants-2010_06