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Acetyl chloride → Ethyl 5-nitro-1,2-benzisothiazole-3-acetate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetyl chloride | HCID 6367 | — |
| 反応物 | Ethyl alpha-cyano-5-nitro-1,2-benziso-thiazole-3-acetate | HCID 12607115 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Ethyl 5-nitro-1,2-benzisothiazole-3-acetate | HCID 18314495 | 17.1% |
反応手順
Ethyl α-cyano-5-nitro-1,2-benzisothiazole-3-acetate (6.67 g, 0.0229 mol) is added to a solution of acetyl chloride (67.0 mL) in ethanol. The reaction mixture is refluxed overnight, cooled, and filtered to remove solids. The resultant filtrate is concentrated in vacuo to obtain a brown semi-solid. A mixture of the semi-solid in diethyl ether is stirred for two hours and filtered to obtain a solid. The solid is washed with diethyl ether and air-dried to give the title product as yellow crystals (1.04 g, mp 91-92° C.).
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-ac498fb1ab074601bb817b4c06e43537 |
| 出典メモ | uspto-grants-2004_03 |