関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 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, 2-methyl-1-octyl- | HCID 170708 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 触媒 | Calcium Chloride | HCID 5284359 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | furo(3,4-b)pyridin-5(7H)-one | HCID 819439 | 279.6% |
反応手順
1.5 g of quinolinic anhydride, 2.3 g of N-octyl-2-methylindole, 10 ml of glacial acetic acid and a mixture of 0.11 g of calcium chloride and 0.14 g of zinc chloride are stirred at 20° C. for 5 hours. 1.6 g of 3-diethylaminophenetole and 2 ml of acetic anhydride are then added, after which the reaction mixture is stirred at 50° C. for 21/2 hours. The product is precipitated with 30% aqueous ammonia, separated from the aqueous phase and recrystallised from isopropanol, affording 3.8 g of the isomer-free 4-azaphthalide compound of the formula (12) of melting point 114°-117° 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-d5dcf0b464df47328f34522762d0d446 |
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| 出典メモ | uspto-grants-1986_05 |
|---|
