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Lithium Hydroxide → 3-Amino-4-phenoxy-5-sulfamoylbenzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Lithium Hydroxide | HCID 3939 | — |
| 反応物 | 3-(Aminosulfonyl)-5-nitro-4-phenoxybenzoic acid | HCID 119926 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3-Amino-4-phenoxy-5-sulfamoylbenzoic acid | HCID 119927 | — |
反応手順
A suspension of 3-nitro-4-phenoxy-5-sulphamyl-benzoic acid (20 g) in water (100 ml) was adjusted to a pH of 8 by the addition of 1N lithium hydroxide. The resulting solution was hydrogenated at room temperature and 1.1 atmosphere hydrogen pressure, using a palladium-on-carbon catalyst (0.6 g catalyst containing 10% pd). After the hydrogen uptake had become negligible, the catalyst was removed by filtration, and the 3-amino- 4-phenoxy-5-sulphamyl-benzoic acid was precipitated from the filtrate by the addition of 4N hydrochloric acid until the pH was 2.5. After recrystallization from aqueous ethanol and drying, the melting point was 255°-256°C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US03971819 |
| 出典データセット | uspto-grants-1976_07 |
| ORD ID | ord-6e8efe1a28ff414796e2748bc3b877ca |
| 出典メモ | uspto-grants-1976_07 |