関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | Acetic Anhydride | HCID 7918 | — |
| 反応物 | Furo[3,4-b]pyridine-5,7-dione | HCID 69688 | — |
| 反応物 | N,N-Diethyl-m-phenetidine | HCID 74625 | — |
| 反応物 | 1H-Indole, 1-ethyl-2-methyl- | HCID 170432 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Isopropanol | HCID 3776 | — |
| 生成物 | furo(3,4-b)pyridin-5(7H)-one | HCID 819439 | 258.8% |
反応手順
20.0 g of quinolinic anhydride, 80 ml of acetic acid, 20.3 g of N-ethyl-2-methylindole and 2.74 g of zinc chloride are stirred at 20° C. for 5 hours. 23.6 g of 3-(N,N-diethylamino)-phenetole and 30 ml of acetic anhydride are then added, after which the reaction mixture is warmed to 50° to 60° C. and stirred at this temperature for 2 hours. After addition of 170 ml of 30% aqueous ammonia and 100 ml of water, the product precipitates as a paste and is isolated. 160 ml of isopropanol are added to the paste and the mixture is refluxed for 1 hour. After cooling, the recrystallised product is filtered off, washed with isopropanol and dried, affording 46.9 g of the isomer-free 4-azaphthalide compound of the formula ##STR15## of melting point 156° to 158° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04587539 |
|---|
| 出典データセット | uspto-grants-1986_05 |
|---|
| ORD ID | ord-96ff3c0d8cde44bca4cbc6c9fb34e7c3 |
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| 出典メモ | uspto-grants-1986_05 |
|---|
