関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Stannous chloride dihydrate | HCID 61436 | — |
| 反応物 | 1H-Indole-2,3-dione, 6-bromo- | HCID 95716 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Sodium Hydroxide | HCID 14798 | — |
| 生成物 | 6-Bromo-1H-indazole-3-carboxylic acid | HCID 24728028 | 169.3% |
反応手順
The solution of 6-bromoisatin (10 g, 22 mmol) in 1N aqueous NaOH solution (48 Ml) was stirred at 50° C. for 1 h. The mixture was cooled to 0° C. Sodium nitrite (3 g, 22 mmol) solution in water (11 Ml) was added dropwise for 15 min at 0° C. The mixture was added to the solution of water (90 Ml) and sulfuric acid (4.6 Ml) at 0° C. for 15 min. The mixture was added to the solution of conc. hydrochloric acid (40 Ml) and SnCl2.2H2O (24 g, 53 mmol). After 1 h, the mixture was filtered and washed with water. The solid was dried through air flow to give the titled compound (8.98 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08754209B2 |
|---|
| 出典データセット | uspto-grants-2014_06 |
|---|
| ORD ID | ord-ea057a89e8594ee181d07db68154d2d4 |
|---|
| 出典メモ | uspto-grants-2014_06 |
|---|
