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Sodium Carbonate → ethyl 5,7-dihydro-6H-dibenz[c,e]azepine-6carboximidate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Triethyloxonium tetrafluoroborate | HCID 2723982 | — |
| 反応物 | 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboxamide | HCID 20041714 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | ethyl 5,7-dihydro-6H-dibenz[c,e]azepine-6carboximidate | HCID 19833914 | — |
反応手順
1.19 g of 5,7-dihydro-6H-dibenz[c,e]azepine-6-carboxamide are dissolved in 10 ml of methylene chloride, and the solution is treated with 1.14 g of triethyloxonium tetrafluoroborate and stirred at room temperature for 20 hours. The mixture is then poured on to 10% sodium carbonate solution/ice and the whole is extracted with methylene chloride. The combined extracts are washed with 10% sodium carbonate solution, dried over anhydrous sodium sulphate and evaporated under reduced pressure. In this manner there is obtained crude ethyl 5,7-dihydro-6H-dibenz[c,e]azepine-6-caboximidate which is purified by a filtration on silica gel [eluent: n-hexane/ethyl acetate (1:1)]; m.p. 74°-76° C. (crystallized from n-hexane).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04766115 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-62a3a9f5b00e4b3493aa4800d32f3db5 |
| 出典メモ | uspto-grants-1988_08 |