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Benzoic acid, 3-sulfo- → 3-(2-Methyl-propane-1-sulfonyl)-benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzoic acid, 3-sulfo- | HCID 8477 | — |
| 反応物 | Isobutyl iodide | HCID 10556 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 3-(2-Methyl-propane-1-sulfonyl)-benzoic acid | HCID 22397459 | — |
反応手順
To a suspension of 3-sulfo-benzoic acid (1 g) and potassium carbonate (1.2 g) in dimethylacetamide (10 ml) was added iso-butyl iodide (0.65 ml). The mixture was heated by microwaves (600W) at 150° C. for 15 minutes. The reaction mixture was partitioned between water (100 ml) and ethyl acetate (100 ml), the aqueous layer was separated, acidified to pH 1 with HCl (2N) and extracted with ethyl acetate (100 ml). The extract was evaporated to leave a residue which was purified by flash chromatography (Biotage 12S eluting with ethyl acetate:hexane:acetic acid, 29:70:1) to give the title product as a white solid (0.34 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06903115B2 |
| 出典データセット | uspto-grants-2005_06 |
| ORD ID | ord-b48b68a8e05c489097e794625cace919 |
| 出典メモ | uspto-grants-2005_06 |