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HRID 65262作成日:2026年10月23日

Triethylamine → alpha-(o-Fluorobenzoylthiomethyl)-beta-phenyl-gamma-butyrolactone

https://huagongshe.com/ja/reaction/65262

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物2-Fluorobenzoic acidHCID 9935—
反応物P,P-Diphenylphosphinic azideHCID 199401—
反応物alpha-Mercaptomethyl-beta-phenyl-gamma-butyrolactoneHCID 13518975—
溶媒Diethyl EtherHCID 3283—
溶媒DimethylformamideHCID 6228—
生成物alpha-(o-Fluorobenzoylthiomethyl)-beta-phenyl-gamma-butyrolactoneHCID 1351891867.2%

反応手順

To a solution of 1.2 g of o-fluorobenzoic acid and 1.5 g of α-mercaptomethyl-β-phenyl-γ-butyrolactone in 20 ml of dimethylformamide were added 1.9 ml of diphenylphosphoryl azide (DPPA) and then 1.2 ml of triethylamine under ice-cooling. Then, the mixture was raised to a room temperature and stirred for 18 hours. After completion of the reaciton, the reaction mixture was diluted with 200 ml of ethyl ether, washed with 5% hydrochloric acid, saturated aqueous sodium hydrogencarbonate, and saturated saline, dried over magnesium sulfate and the solvent was then distilled off. The crude product thus obtained was purified by a silica gel column chromatography to give 1.6 g (yield 67%) of the title compound.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04613613
出典データセットuspto-grants-1986_09
ORD IDord-0a89f202a1ce4947b408e89c52abab67
出典メモuspto-grants-1986_09