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HRID 329044作成日:2026年10月25日

Triethylamine → Flupimazine

https://huagongshe.com/reaction/329044

反応式

関与物質

役割名称HCID仕込み量
反応物TriethylamineHCID 8471—
反応物10-(3-Chloropropyl)-2-(trifluoromethyl)-10H-phenothiazineHCID 74294—
反応物2-(Piperidin-4-yloxy)ethan-1-olHCID 20295332—
溶媒Sodium IodideHCID 5238—
溶媒Methyl Ethyl KetoneHCID 6569—
生成物FlupimazineHCID 218089—

反応手順

40 g of 2-trifluoromethyl-10-(3-chloropropyl)-phenothiazine were dissolved in 350 ml of methyl ethyl ketone and 17.6 g of sodium iodide, 11.8 g of triethylamine, then 17 g of 2-(4-piperidyloxy)-ethanol were successively added to this solution. It was refluxed for 20 hours and after cooling, the precipitate was removed by vacuum filtration. The filtrate was evaporated to dryness to obtain 2-trifluoromethyl-10-[3-(4-β-hydroxyethoxypiperidino)-propyl]-phenothiazine as an oil which was added to a mixture of ether and dilute hydrochloric acid. The formed precipitate was recovered by vacuum filtration and was crystallized from 95% ethanol to obtain 40.5 g of 2-trifluoromethyl-10-[-3(4-β-hydroxyethoxypiperidino)-propyl]-phenothiazine hydrochloride as white crystals. Then a current of ammonia was led into an ether suspension of this product and the formed precipitate was removed by filtration. The filtrate was evaporated to dryness to obtain 2-trifluoromethyl-10-[3-(4-β-hydroxyethoxypiperidino)-propyl]-phenothiazine as an oil.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04018922
出典データセットuspto-grants-1977_04
ORD IDord-44caedd389744c3aa62118cfbc87512f
出典メモuspto-grants-1977_04