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Thionyl Chloride → 7-Nitro-1,4-benzodioxane-5-carbonyl chloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thionyl Chloride | HCID 24386 | — |
| 反応物 | 7-Nitro-2,3-dihydro-1,4-benzodioxine-5-carboxylic acid | HCID 12464533 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 7-Nitro-1,4-benzodioxane-5-carbonyl chloride | HCID 20544745 | 100% |
反応手順
112 ml of thionyl chloride, 56 g of 7-nitro-1,4-benzodioxane-5-carboxylic acid were introduced into a 250 ml balloon flask provided with a stirrer, a thermometer and a reflux condenser. The mixture was stirred and 1 ml of dimethylformamide was added with heating. After stirring for one hour at the reflux temperature, the excess of thionyl chloride was removed by distillation under vacuum. 61 g of 7-nitro-1,4-benzodioxane-5-carbonyl chloride were obtained (M.P.: 108° C.; yield: 100%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04306072 |
| 出典データセット | uspto-grants-1981_12 |
| ORD ID | ord-ce9ca5fa176d48f8b83c69e1998b2ee5 |
| 出典メモ | uspto-grants-1981_12 |