化工社化工社 化学情報印刷レポート · 研究参考用
Nitric Acid → Ethyl 2-iodo-4-(trifluoromethyl)-5-thiazolecarboxylate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitric Acid | HCID 944 | — |
| 反応物 | Phosphoric Acid | HCID 1004 | — |
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | 5-Thiazolecarboxylic acid, 2-amino-4-(trifluoromethyl)-, ethyl ester | HCID 67656 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | Ethyl 2-iodo-4-(trifluoromethyl)-5-thiazolecarboxylate | HCID 13593392 | 25.7% |
反応手順
To a cold (-5° C.) solution of 4.0 g (0.0166 mole) of ethyl 2-amino-4trifluoromethyl-5-thiazolecarboxylate, prepared according to U.S. Pat. No. 2,726,237, in 30 ml. of 85% phosphoric acid and 30 ml. of 70% nitric acid was added a solution of 1.26 g (0.0166 mole) of sodium nitrite in 10 ml. of water in 10 minutes. The reaction mixture was stirred for 10 minutes and poured into a solution of 10 g of potassium iodide in 100 ml. of water. The reaction mixture was stirred overnight and extracted with ether. The ether solution was dried and concentrated and the residue was chromatographed on silica gel to give 1.5 g of the desired product, m.p. 75°-76° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04586948 |
| 出典データセット | uspto-grants-1986_05 |
| ORD ID | ord-86f4d5e582f24b94b6709ab592ac9bf3 |
| 出典メモ | uspto-grants-1986_05 |