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HRID 660125作成日:2026年10月27日

Pyridine → 2-Methyl-2-nitro-1,3-propanediol ditriflate

https://huagongshe.com/reaction/660125

反応式

関与物質

役割名称HCID仕込み量
反応物PyridineHCID 1049—
反応物2-Methyl-2-nitro-1,3-propanediolHCID 6480—
反応物Trifluoromethanesulfonic anhydrideHCID 67749—
溶媒ChloroformHCID 6212—
生成物2-Methyl-2-nitro-1,3-propanediol ditriflateHCID 59393620—

反応手順

To a solution of triflic anhydride (16.5 ml, 0.1 mol) in chloroform (50 ml) is added a solution of 2-methyl-2-nitro-1,3-propanediol (6.75 g, 0.05 mol) and pyridine (8.85 ml, 0.11 mol) in chloroform (50 ml) with external cooling to ensure a temperature of between 0° and 5° C. during the addition. After the addition the cooling bath is removed and the reaction stirred for 18 hours at ambient temperature. The reaction mixture is transferred to a separating funnel and washed with water. The organic layer is dried (Na2SO4), filtered and evaporated to dryness. The crude product is purified by chromatography using a 4:1 mixture of Hexane:Ethyl acetate as eluant; the product is obtained as a solid with melting point 50-52° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08084474B2
出典データセットuspto-grants-2011_12
ORD IDord-ada0034dde9c449e94832228aecc81c6
出典メモuspto-grants-2011_12