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Ethanolamine → N-[3-(4-tert-butylcyclohexan-1-yl)phenyl]-4-[2-[N-(2-hydroxyethyl)amino]ethoxy]-3-methoxyphenylacetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanolamine | HCID 700 | — |
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 4-(2-bromoethoxy)-N-[3-(4-tert-butylcyclohexan-1-yl)phenyl]-3-methoxyphenylacetamide | HCID 22019627 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | N-[3-(4-tert-butylcyclohexan-1-yl)phenyl]-4-[2-[N-(2-hydroxyethyl)amino]ethoxy]-3-methoxyphenylacetamide | HCID 22019647 | 88.5% |
反応手順
Intermediate 5 (200 mg), 2-aminoethanol (122 mg) and triethylamine (45 mg) are dissolved in acetonitrile (5 ml), and the mixture is heated under reflux for 18 hours. To the reaction solution is added chloroform, and the mixture is washed with water. The organic layer is dried over sodium sulfate, and the solvent is evaporated under reduced pressure. The residue is purified by silica gel column chromatography (eluent: gradient from 0% to 20% chloroform/methanol) to give the desired compound (170 mg).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07084176B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-ca4213a13adb45e8b1ae784052865be6 |
| 出典メモ | uspto-grants-2006_08 |