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Potassium Carbonate → 2-Hydroxy-1,3-benzothiazole-6-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Triphosgene | HCID 94429 | — |
| 反応物 | 4-Amino-3-mercaptobenzoic acid | HCID 598058 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 2-Hydroxy-1,3-benzothiazole-6-carboxylic acid | HCID 14116709 | 95.3% |
反応手順
4-Amino-3-mercaptobenzoic acid (680 mg) was dissolved in tetrahydrofuran (20 ml), and potassium carbonate (550 mg) was added thereto and stirred for 30 minutes at room temperature. The mixture was cooled to −78° C., and triphosgene (400 mg) was added thereto and stirred for 1 hour. The mixture was warmed to room temperature and concentrated under reduced pressure until the volume of the solvent became ⅓. Water (20 ml) and formic acid were added to the concentrate until it became acidic, and precipitated crystals were collected by filtration and washed with water and n-hexane. The crystals were dried under reduced pressure to give the title compound (740 mg, Y.:95%) as white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07345180B2 |
| 出典データセット | uspto-grants-2008_03 |
| ORD ID | ord-94ef4221512d495fbec3be3264be954f |
| 出典メモ | uspto-grants-2008_03 |