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Pyridine → 5-[4-(4-tert-Butyl-phenoxy)-phenylsulfamoyl]-2-methyl-benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | 4-(4-Tert-butylphenoxy)aniline | HCID 82498 | — |
| 反応物 | 5-(Chlorosulfonyl)-2-methylbenzoic acid | HCID 308449 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 5-[4-(4-tert-Butyl-phenoxy)-phenylsulfamoyl]-2-methyl-benzoic acid | HCID 58937040 | 82% |
反応手順
A solution of 4-(4-tert-butyl-phenoxy)-phenylamine (0.1 g, 0.41 mmol). 5-chlorosulfonyl-2-methylbenzoic acid (0.097 g, 0.41 mmol) and pyridine (0.1 ml, 1.24 mmol) in 2 ml anhydrous tetrahydrofuran was heated at 60° C. for 2 hr. The reaction mixture was cooled to room temperature and diluted with 30 ml ethyl acetate. The ethyl acetate solution was washed sequentially with 25 ml 1N aqueous hydrochloric acid solution and 25 ml brine, dried (anhydrous sodium sulfate) and concentrated to dryness under reduced pressure. The crude product was purified by preparative thick layer chromatography (silica gel), eluting with 9:1 chloroform/methanol to yield the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07262318B2 |
| 出典データセット | uspto-grants-2007_08 |
| ORD ID | ord-d16715c87bba49a5856bec6decc7aad8 |
| 出典メモ | uspto-grants-2007_08 |