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Acryloyl chloride → HCID 178460006、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acryloyl chloride | HCID 13140 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | HCID 178478652 | HCID 178478652 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | HCID 178460006 | HCID 178460006 | 58.5% |
反応手順
20.7 g of 5-aminobenzotriazole dihydrochloride and 30 g of sodium hydrogen carbonate were dissolved in 300 ml of water, and 10 g of acryl chloride was added dropwise at a temperature of lower than 10° C. over 20 minutes. After being stirred for 1 hour, the formed white precipitate was filtered off. Yield: 13.8 g. It was dissolved in 100 ml of DMF, and 500 ml of hot water at about 70° C. was added. It was immediately filtered under atmospheric pressure. The filtrate was allowed to cool, and the separated crystals were filtered out, washed with water and dried to obtain 11 g of the desired product which melted at 248°-253° C. The structure was confirmed by IR, NMR and elementary analysis.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04528264 |
| 出典データセット | uspto-grants-1985_07 |
| ORD ID | ord-fd874fcb90364f05b78097c74f8e01c8 |
| 出典メモ | uspto-grants-1985_07 |