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Triethylamine → N-[2-(1-Piperidyl)propyl]-3-methylflavone-8-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Ethyl chloroformate | HCID 10928 | — |
| 反応物 | 3-Methylflavone-8-carboxylic acid | HCID 77016 | — |
| 反応物 | 2-(Piperidin-1-yl)propan-1-amine | HCID 12455409 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | N-[2-(1-Piperidyl)propyl]-3-methylflavone-8-carboxamide | HCID 13388197 | 71.9% |
反応手順
To a solution of 4.00 g of 3-methylflavone-8-carboxylic acid and 1.98 ml of triethylamine in 74 ml of anhydrous tetrahydrofuran was added a solution of 1.50 ml of ethyl chlorocarbonate in 15 ml of anhydrous tetrahydrofuran under ice-cooling and the mixture was stirred for 1 hour. To the mixture, a solution of 2.03 g of 2-piperidinopropylamine in 20 ml of anhydrous tetrahydrofuran was added and the mixture was stirred for 1.5 hours under ice-cooling and further at room temperature for 16 hours. The reaction mixture was treated by the same procedure as in Examples 3(b) to give 4.15 g of colorless crystals, which were recrystallized from ethyl acetate as colorless needles, m.p. 106.5°-108.5° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04525356 |
| 出典データセット | uspto-grants-1985_06 |
| ORD ID | ord-ff73ddac30514135a893d04a371c2dca |
| 出典メモ | uspto-grants-1985_06 |