化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → Ethyl alpha-cyano-5-nitro-1,2-benziso-thiazole-3-acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Ethyl cyanoacetate | HCID 7764 | — |
| 反応物 | 1,2-Benzisothiazole, 3-chloro-5-nitro- | HCID 198098 | — |
| 反応物 | Sodium ethoxide | HCID 2723922 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | Ethyl alpha-cyano-5-nitro-1,2-benziso-thiazole-3-acetate | HCID 12607115 | — |
反応手順
A sodium ethoxide solution (previously prepared from ethanol and sodium (1.00 g, 0.0430 mol)) is cooled with an ice-acetone bath, treated portionwise with ethyl cyanoacetate (4.51 g, 0.0398 mol), stirred at room temperature for 30 minutes, treated with 3-chloro-5-nitro-1,2-benzisothiazole (4.27 g, 0.0199 mol), stirred at room temperature overnight, cooled to 0° C., and treated dropwise with 10% hydrochloric acid (15.0 mL). The resultant mixture is stirred at room temperature for one hour and filtered to obtain a solid. The solid is washed with ethanol and air-dried to give the title product as a yellow solid which is identified by NMR spectral analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06706663B2 |
| 出典データセット | uspto-grants-2004_03 |
| ORD ID | ord-85bb76098ecc416382d1dfad51bbdc70 |
| 出典メモ | uspto-grants-2004_03 |