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HRID 592536作成日:2026年10月27日

Water → 3,4,5,6,7,8-Hexahydrobenzo[4,5]thieno[2,3-c]pyridin-1(2H)-one

https://huagongshe.com/reaction/592536

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物5,6,7,8-Tetrahydro-1H-benzo[b]cyclopenta[d]thiophen-3(2H)-one OximeHCID 76671726—
生成物3,4,5,6,7,8-Hexahydrobenzo[4,5]thieno[2,3-c]pyridin-1(2H)-oneHCID 2089975475%

反応条件

温度80 °C

反応手順

A 50-mL single-neck round-bottomed flask equipped with a reflux condenser, magnetic stirrer and nitrogen inlet was charged with 105d (285 mg, 1.38 mmol) and polyphosphoric acid (15 g). After stirring at 80° C. for 16 h, the reaction mixture was cooled to room temperature, and water (30 mL) was added. The resulting mixture was stirred for 30 min and filtered. The filter cake was washed with water (20 mL) and dried in a vacuum oven at 45° C. to afford a 75% yield (215 mg) of 105e as an off-white solid: mp 203° C. dec; 1H NMR (500 MHz, CDCl3) δ 5.62 (s, 1H), 3.59 (t, 2H, J=7.0 Hz), 2.81 (t, 2H, J=6.0 Hz), 2.72 (t, 2H, J=7.0 Hz), 2.48 (t, 2H, J=6.0 Hz), 1.84 (m, 4H). MS (APCI+) m/z 208.3 (M+H)

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US09238655B2
出典データセットuspto-grants-2016_01
ORD IDord-fbdfb07e7c7b49c1a13a96b3e8edb407
出典メモuspto-grants-2016_01