関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methoxyphenol | HCID 9015 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Benzo(b)thiophene, 3-bromo- | HCID 123250 | — |
| 触媒 | Copper(1+) iodide; Copper(I) iodide; Cuprous iodide; Cuprous iodide (CuI) | HCID 24350 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-(4-Methoxyphenoxy)benzo[b]thiophene | HCID 10824975 | — |
反応手順
A mixture of 4.00 g (19.7 mmol) of 3-bromobenzo[b]thiophene, 4.96 g (40 mmol) of 4-methoxyphenol, 5.52 g (40 mmol) of K2CO3, and 0.20 g (1.0 mmol) of CuI was heated to 140° C. and sonicated at this temperature for 2 h. The reaction was allowed to cool, taken up in CH2Cl2, and the mixture was washed several times with 0.5 N NaOH. The organic layer was dried over Na2SO4 and concentrated in vacuo to an oil that was subjected to chromatography (SiO2; gradient of 0-5% EtOAc in hexanes). The fractions containing the desired product were combined, evaporated in vacuo, and the residue was recrystallized from hexanes to afford 500 mg (1.95 mmol; 10%) of the title compound as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06265575B1 |
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| 出典データセット | uspto-grants-2001_07 |
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| ORD ID | ord-88fa74840acb457dbd2585d04240b8d3 |
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| 出典メモ | uspto-grants-2001_07 |
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