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HRID 376971作成日:2026年10月25日

Water → 1-[4-(4-Mercaptobutylthio)-phenyl]-2-methyl-2-morpholin-4-yl-propan-1-one

https://huagongshe.com/reaction/376971

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Potassium CarbonateHCID 11430—
反応物1,4-ButanedithiolHCID 79148—
反応物1-(4-Chlorophenyl)-2-methyl-2-(morpholin-4-yl)propan-1-oneHCID 15702408—
溶媒DimethylacetamideHCID 31374—
生成物1-[4-(4-Mercaptobutylthio)-phenyl]-2-methyl-2-morpholin-4-yl-propan-1-oneHCID 19360615—

反応手順

40 g (0.15 mol) of 1-(4-chlorophenyl)-2-methyl-2-morpholin-4-yl-propan-1-one and 109 g (0.89 mol) of 1,4-butanedithiol are dissolved in 300 ml of dimethylacetamide, and the solution is stirred at around 100° C. together with 41 g of potassium carbonate for 5 h. Then the solution is cooled to room temperature and poured into water. The crude product is extracted with ethyl acetate, washed with saturated sodium chloride solution, dried over MgSO4, and concentrated. The residue is purified by column chromatography on silica gel with ethyl acetate -hexane (20:80) as an eluent. Melting point 98 ° C. The structure is confirmed by the 1H-NMR spectrum (CDCl3): δ [ppm] 1.31 (s, 6H), 1.36 (t, 1H), 1.76-1.90 (m, 4H), 2.53-2.62 (m, 6H), 2.98-3.04 (m, 2H), 3.69 (t, 4H), 7.25 (d, 2H), 8.50 (d, 2H).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06022906
出典データセットuspto-grants-2000_02
ORD IDord-179104a951b34286bb7623e5ec05b593
出典メモuspto-grants-2000_02