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Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) → N-Methyl-N-tert-butoxycarbonyl-2-(3,4-dichlorophenyl)-2-(2-hydroxyethoxy)ethanamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Benzenesulfonic acid, 4-methyl-, compd. with pyridine (1:1) | HCID 466102 | — |
| 反応物 | N-Methyl-N-tert-butoxycarbonyl-2-(3,4-dichlorophenyl)-2-[2-(tetrahydropyran-2-yloxy)ethoxy]ethanamine | HCID 19692483 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | N-Methyl-N-tert-butoxycarbonyl-2-(3,4-dichlorophenyl)-2-(2-hydroxyethoxy)ethanamine | HCID 19692490 | 100.9% |
反応手順
0.56 g of pyridinium paratoluenesulfonate is added to a solution of 10 g of the compound obtained in EXAMPLE 8, step C), in 100 ml of MeOH and the reaction mixture is refluxed for 1 hour 15 minutes. It is concentrated under vacuum and the residue is taken up with ether, washed with water and with a buffer solution of pH 2, dried over MgSO4 and concentrated under vacuum to give 8.2 g of the expected product, which is used as such in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05726313 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-c7a3ca41e01d4efebb1bd0e9b36a8939 |
| 出典メモ | uspto-grants-1998_03 |