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HRID 2390573作成日:2026年10月25日

Ethanol → HCID 58120259、化合物

https://huagongshe.com/reaction/2390573

反応式

関与物質

役割名称HCID仕込み量
反応物EthanolHCID 702—
反応物Sodium hydrideHCID 24758—
反応物Benzene, 2,4-dichloro-1-fluoro-HCID 123112—
反応物(S)-3-((R)-1-Hydroxy-2-isopropoxyethyl)pyrrolidine-1-carboxylic Acid t-Butyl EsterHCID 66859524—
溶媒Hydrochloric AcidHCID 313—
溶媒DimethylformamideHCID 6228—
生成物HCID 58120259HCID 58120259—

反応手順

(S)-3-((R)-1-Hydroxy-2-isopropoxyethyl)pyrrolidine-1-carboxylic acid t-butyl ester (25.0 mg, 91.4 μmol) was dissolved in DMF (190 μL). NaH (2.6 mg, 109.7 μmol) was added and the mixture was stirred at room temperature for 15 minutes. 2,4-Dichloro-1-fluorobenzene (21.4 μL, 182.9 μmol) was added and the mixture was stirred at 70° C. for 3 hours. The mixture was concentrated then dissolved in 1.2M HCl in EtOH (949 μL, 1.1 mmol) and stirred overnight. The product was concentrated and purified by preparative HPLC to yield the title compound as a mono-TFA salt oil (29.5 mg, 97% purity). MS m/z: [M+H]+ calcd for C15H21Cl2NO2, 318.10; found 318.0.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08273786B2
出典データセットuspto-grants-2012_09
ORD IDord-d0155b85e18b47a59df911bc2a7eee0a
出典メモuspto-grants-2012_09