化工社化工社 化学情報印刷レポート · 研究参考用
Cyclopropylamine → HCID 178418548、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Cyclopropylamine | HCID 69828 | — |
| 反応物 | Ethylorthoformate | HCID 53630039 | — |
| 反応物 | Ethyl 2,5-difluoro-4-(pyrrol-1-yl)benzoylacetate | HCID 53691688 | — |
| 溶媒 | Acetic Anhydride | HCID 7918 | — |
| 生成物 | HCID 178418548 | HCID 178418548 | 36.1% |
反応手順
1 g (0.0068 mol) of ethyl orthoformate is added to a solution of 1.1 g (0.00315 mol) of ethyl 2,5-difluoro-4-(pyrrol-1-yl)benzoylacetate in 3 ml of acetic anhydride and the mixture is refluxed for 3 hours. It is evaporated to dryness, the residue is dissolved in 10 ml of ethanol, 0.3 ml (0.0034 mol) of cyclopropylamine is added and the mixture is left at room temperature for 1 hour. It is evaporated to dryness and the oily residue is extracted with 3×30 ml of boiling hexane. The hexane fractions are concentrated to 20 ml and left for 12 hours at 5° C. to give 0.41 g of crystals melting at 90°-2° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04727080 |
| 出典データセット | uspto-grants-1988_02 |
| ORD ID | ord-a4b80bde42b64cf99f5959c49c2e964f |
| 出典メモ | uspto-grants-1988_02 |