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HRID 4813作成日:2026年10月23日

Lawesson's reagent → 2-(2-Chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-thiazepine-5(4H)-thione

https://huagongshe.com/ja/reaction/4813

反応式

関与物質

役割名称HCID仕込み量
反応物Lawesson's reagentHCID 87949—
反応物2-(2-Chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-thiazepin-5(4H)-oneHCID 13726457—
溶媒TolueneHCID 1140—
生成物2-(2-Chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]-thiazepine-5(4H)-thioneHCID 13726458—

反応手順

A mixture of 4.3 g (0.017 mole) of 2-(2-chloroethyl)-2,3-dihydro-4-methylpyrido[3,2-f][1,4]thiazepin-5(4H)-one, 100 ml of toluene and 4.8 g (0.012 mole) of 2,4-bis(4-methoxyphenyl)-1,3,2,4-dithiadiphosphetane-2,4-disulfide was refluxed for 3 hr and then extracted twice with dilute sodium hydroxide. The organic layer was concentrated and the residue chromatographed on the high pressure liquid chromatograph using a silica column and 50% ethyl acetate-50% hexane. The yield of title compound was 2 g, m.p. 160°-162° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04727152
出典データセットuspto-grants-1988_02
ORD IDord-2835159553ab4fcdb331894bd71cc090
出典メモuspto-grants-1988_02