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Hydrochloric Acid → 5-Chlorobenzo[b]thiophene-3-methanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Potassium Acetate | HCID 517044 | — |
| 反応物 | 3-(Bromomethyl)-5-chloro-1-benzothiophene | HCID 2779857 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | 5-Chlorobenzo[b]thiophene-3-methanol | HCID 2776136 | — |
反応手順
A solution of 3-bromomethyl-5-chlorobenzothiophene (2.5 g, 9.56 mmol) and potassium acetate (1.96 g, 20 mmol) in 1M NaOH (40 mL) and dioxane (40 mL) was heated to reflux for 24 hours, adjusted to pH<7 with 1M HCl, and extracted with ethyl acetate (3×). The combined extracts were washed with brine, concentrated, and purified by flash column chromatography on silica gel with 50% ethyl acetate/hexanes to provide the desired product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07754886B2 |
| 出典データセット | uspto-grants-2010_07 |
| ORD ID | ord-d210905a0a054a28b97763d8185b9170 |
| 出典メモ | uspto-grants-2010_07 |