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HRID 476934作成日:2026年10月26日

Oxalic Acid → 5-[2-[4[Bis(4-fluorophenyl)hydroxymethyl]-1-piperidinyl]ethyl]-3-methyl-2-oxazolidinone oxalate

https://huagongshe.com/reaction/476934

反応式

関与物質

役割名称HCID仕込み量
反応物Oxalic AcidHCID 971—
反応物Potassium IodideHCID 4875—
反応物Sodium CarbonateHCID 10340—
反応物Bis(4-fluorophenyl)(piperidin-4-yl)methanolHCID 11208889—
反応物5-(2-Chloro-ethyl)-3-methyl-oxazolidin-2-oneHCID 14698746—
溶媒1-ButanolHCID 263—
生成物5-[2-[4[Bis(4-fluorophenyl)hydroxymethyl]-1-piperidinyl]ethyl]-3-methyl-2-oxazolidinone oxalateHCID 1983672271%

反応手順

A mixture of 3.0 g (0.01 mole) of α,α-bis(p-fluorophenyl)-4-piperidinemethanol, 1.6 g (0.01 mole) of 5-(2-chloroethyl)-3-methyl-2-oxazolidinone, 5.3 g (0.085 mole) of anhydrous sodium carbonate and 0.3 g of potassium iodide in 100 ml of 1-butanol was heated at reflux for 20 hr. The mixture was concentrated under reduced pressure and the residue was partitioned between water and benzene. The benzene layer was washed with water and brine, dried over anhydrous sodium sulfate and concentrated under reduced pressure to give a gum as residue. The gum was converted to the oxalic acid salt, recrystallizing from absolute ethanol to give 3.7 g (71%) of white powder, m.p. 124°-134° C. with decomposition.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04886794
出典データセットuspto-grants-1989_12
ORD IDord-e650102e8b3d4db68039db5dbc670305
出典メモuspto-grants-1989_12