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Sulfuric Acid → 1-Iodo-4-nitro-2-(trifluoromethyl)benzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | 4-Nitro-alpha,alpha,alpha-trifluoro-o-toluidine | HCID 67128 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Iodo-4-nitro-2-(trifluoromethyl)benzene | HCID 19261778 | 94.6% |
反応手順
To a mixture of 3.1 g (15.0 mmol) of 2-amino-5-nitrobenzotrifluoride in 60 mL of 40% (v/v) H2SO4 stirred in an ice-bath was added dropwise a solution of 2.1 g (30.4 mmol) of NaNO2 in 10 mL of H2O. The resulting yellow solution was stirred in an ice-bath for 1 h and it was added dropwise into a well stirred solution of 10 g of NaI in 250 mL of H2O cooled in an ice bath. Gas releasing and precipitate was observed. The mixture was stirred overnight at 25° C., filtered and washed by water, and dried to leave pale yellow solid (4.5 g, 94%), mp 81°-82° C. 1H NMR (CDCl3), 8.047 (dd, 1), 8.272 (d, 1), 8.483 (d, 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05622952 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-927e014c875c4451a486c552d6849f30 |
| 出典メモ | uspto-grants-1997_04 |