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1-Ethynylcyclohexylamine → 1-[2-Cyano-4-(isobutyroyl-amino)-phenoxy]-3-(1-ethinyl-cyclohexylamino)-2-propanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Ethynylcyclohexylamine | HCID 121691 | — |
| 反応物 | 1-[2-Cyano-4-(isobutyroyl-amino)-phenoxy]-2,3-epoxy-propane | HCID 23318127 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 1-[2-Cyano-4-(isobutyroyl-amino)-phenoxy]-3-(1-ethinyl-cyclohexylamino)-2-propanol | HCID 12939913 | — |
反応手順
7.8 gm (0.03 mol) of 1-[2-cyano-4-(isobutyroyl-amino)-phenoxy]-2,3-epoxy-propane were dissolved in 80 ml of ethanol, and after addition of 7.5 gm (0.06 mol) of 1-ethinyl-cyclohexyl-amine the mixture was refluxed for one hour. The solvent was then distilled off, and the residue was acidified with dilute HCl. After extraction with ethyl acetate the aqueous phase was made alkaline by addition of NaOH, whereby basic components precipitated in oily form. They were taken up in ethyl acetate, the organic phase was washed with water, dried over MgSO4, evaporated and the solid residue was recrystallized twice from acetonitrile.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04344964 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-1bc5ffdd6ad2418a94a352058c4ea0a0 |
| 出典メモ | uspto-grants-1982_08 |