関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Pyrrolidine | HCID 31268 | — |
| 反応物 | [7-(Methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methyl 4-methylbenzenesulfonate | HCID 86652933 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 44469455 | HCID 44469455 | — |
反応手順
A mixture of [7-(methylsulfonyl)-2,3-dihydro-1,4-benzodioxin-2-yl]methyl 4-methylbenzenesulfonate (0.4 g, 0.9 mmol), pyrrolidine (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 twice on flash column chromatography (Isooctane/EtOAc/MeOH). Yield: 0.2 g, 75%. The amine was converted to the hydrochloric acid salt and crystallized from MeOH/Et2O. M.p. 221° C. MS m/z (rel. intensity, 70 eV) 297 (M+, 1), 85 (6), 84 (bp), 79 (2), 55 (4).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08524766B2 |
|---|
| 出典データセット | uspto-grants-2013_09 |
|---|
| ORD ID | ord-06f1855b5e26442d8dd650b36086854b |
|---|
| 出典メモ | uspto-grants-2013_09 |
|---|
