関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Benzoic acid, 3-(chlorosulfonyl)- | HCID 77641 | — |
| 反応物 | 2-(Chlorosulfonyl)benzoic acid | HCID 14474464 | — |
| 溶媒 | O-Xylene | HCID 7237 | — |
| 生成物 | Benzoic acid, 3-sulfo- | HCID 8477 | 95.6% |
反応手順
300 g of 3-(chlorosulfonyl)benzoic acid containing 38.8% water (corresponding to 183.6 g (0.83 mol) of 100% chlorosulfonylbenzoic acid) are admixed with 150 g of water and heated at 100° C. for 1 hour. Then 600 g of xylene are added dropwise over 1 hour and a total of 260 ml of water are azeotropically distilled off with xylene. The reaction mixture is cooled and the precipitate is filtered off with suction. After drying at 100° C./100 torr (13.16 kPa) 164.7 g of 3-sulfobenzoic acid are obtained, the purity determined by titration being 97.7%; this corresponds to a yield of 95.6%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05387711 |
|---|
| 出典データセット | uspto-grants-1995_02 |
|---|
| ORD ID | ord-5c21ac4fce2b41ce973bccab5db1a867 |
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| 出典メモ | uspto-grants-1995_02 |
|---|
