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Hydrochloric Acid → 4-(3,4-Dichloro-benzenesulfonyl)-piperidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Tert-butyl 4-[(3,4-dichlorophenyl)sulfonyl]piperidine-1-carboxylate | HCID 68550800 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-(3,4-Dichloro-benzenesulfonyl)-piperidine | HCID 22397499 | 79.3% |
反応手順
A mixture of the sulfone from Step 7C (3.09 g, 7.8 mmol), MeOH (21 mL), and 5N HCl (4.5 mL) was heated to reflux for 1.5 h. The mixture was cooled to room temperature and sat. Na2CO3 solution (80 mL) was added. The mixture was extracted with CH2Cl2 (2×100 mL). The organic phase washed with H2O and brine, dried (MgSO4) and concentrated to afford the amine (1.82 g), a white foam, in 79% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07632838B2 |
| 出典データセット | uspto-grants-2009_12 |
| ORD ID | ord-432e23b2e5314003886ac50bc41be741 |
| 出典メモ | uspto-grants-2009_12 |