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Methanamine, N-methoxy-, hydrochloride (1:1) → 3-tert-Butyl-N-methoxy-N-methyl-5-[3-(tetrahydropyran-2-yloxy)propoxy]benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methanamine, N-methoxy-, hydrochloride (1:1) | HCID 81138 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | O-[(Ethoxycarbonyl)cyanomethylenamino]-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733286 | — |
| 反応物 | 3-tert-Butyl-5-[3-(tetrahydropyran-2-yloxy)propoxy]benzoic acid | HCID 58136832 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-tert-Butyl-N-methoxy-N-methyl-5-[3-(tetrahydropyran-2-yloxy)propoxy]benzamide | HCID 58136958 | 99.4% |
反応手順
3-tert-Butyl-5-[3-(tetrahydropyran-2-yloxy)propoxy]benzoic acid (O4.059; 4.90 g) and N,O-dimethylhydroxylaminehydrochloride (1.42 g) were dissolved in DMF (80 ml) and admixed with Hünig's base (4.81 ml) and TOTU (4.78 g). After stirring for 2 h, the mixture was left to stand overnight. Then the DMF was drawn off, the mixture was partitioned between EA and saturated sodium hydrogencarbonate solution, and the EA phase was removed, dried over magnesium sulfate, filtered and concentrated. 5.49 g of the title compound were obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08198272B2 |
| 出典データセット | uspto-grants-2012_06 |
| ORD ID | ord-aa8b3e8f1c4a4b8c90256da1b6eea2b5 |
| 出典メモ | uspto-grants-2012_06 |