関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 2-Thiophenethiol | HCID 522674 | — |
| 反応物 | 1-(Diphenylmethyl)azetidin-3-yl methanesulfonate | HCID 2758716 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-Benzhydryl-3-(thiophen-2-ylthio)-azetidine | HCID 67154611 | — |
反応手順
Potassium hydroxide (141 mg, 2.52 mmol) and thiophene-2-thiol (292 mg, 238 μL) were added to a solution of 1-benzhydrylazetidin-3-yl methanesulfonate (400 mg, 1.26 mmol) solubilized in THF (7 mL). The reaction mixture was stirred a first time under microwave irradiations (100 W) at 80° C. for 30 minutes. Potassium hydroxide (141 mg, 2.52 mmol) and thiophene-2-thiol (292 mg, 238 μL) were added and the reaction mixture was stirred for a second time under microwave irradiations (100 W) at 80° C. for 30 minutes. After concentration to dryness, the residue was purified by chromatography on silica gel using petroleum ether/ethyl acetate (1:0 to 9:1) as eluent. The title product was obtained as a yellow solid (160 mg, 37%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08846711B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-ad9462dac0964153bcf443371ef3345c |
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| 出典メモ | uspto-grants-2014_09 |
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