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HRID 903653作成日:2026年10月25日

Water → 2-Hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin

https://huagongshe.com/reaction/903653

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物Sodium HydroxideHCID 14798—
反応物2-Methoxy-9-cyano-10,11-dihydrodibenzo[b,f]thiepinHCID 23337048—
溶媒Diethylene GlycolHCID 8117—
生成物2-Hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepinHCID 2333704146%

反応条件

温度200 °C

反応手順

An amount of 2.2 g of sodium hydroxide was dissolved in 30 ml of diethylene glycol by application of heat and to the mixture was added 2.2 g of 2-methoxy-9-cyano-10,11-dihydrodibenzo[b,f]thiepin and the resulting mixture was stirred at 200° C. for 16 hours. After cooling, to the mixture was added water and the mixture was extracted with ethyl acetate. The aqueous layer was acidified with conc. hydrochloric acid and extracted with ethyl acetate. This extract was washed with saturated sodium chloride solution, dried over anhydrous sodium sulfate and freed of the solvent to obtain the residue. This residue was recrystallized from benzene to afford 1.1 g (46%) of 2-hydroxy-9-carboxy-10,11-dihydrodibenzo[b,f]thiepin as brown crystals having a melting point of 210°-211° C.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US04228284
出典データセットuspto-grants-1980_10
ORD IDord-603a21f55369406e860621300fd1d1fb
出典メモuspto-grants-1980_10