関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Propylamine | HCID 7852 | — |
| 反応物 | [(2R)-7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methyl 4-methylbenzenesulfonate | HCID 86652935 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 44469324 | HCID 44469324 | — |
反応手順
A mixture of [(2R)-7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methyl 4-methylbenzenesulfonate (0.4 g, 0.9 mmol), propan-1-amine (1 ml) and ACN (3 ml) was heated under microwave radiation at 120° C. for 20 min. Purification on SCX-3 column (TEA/MeOH) and on a small silica plug (DCM/MeOH). Yield: 0.2 g, 90%. The amine was converted to the hydrochloric acid salt and crystallized from MeOH/Et2O. M.p. 228° C. MS m/z (rel. intensity, 70 eV) 285 (M+, 2), 79 (3), 73 (5), 72 (bp), 70 (5). [α]=−73° (MeOH).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08524766B2 |
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| 出典データセット | uspto-grants-2013_09 |
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| ORD ID | ord-4a7a17826fb24594ada19f3c90f6e49c |
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| 出典メモ | uspto-grants-2013_09 |
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