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Ammonia → 1-[5-Chloro-2-(methylsulfonyl)phenyl]methanamine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ammonia | HCID 222 | — |
| 反応物 | 5-Chloro-2-(methylsulfonyl)benzonitrile | HCID 66970048 | — |
| 触媒 | Cobalt | HCID 104730 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-[5-Chloro-2-(methylsulfonyl)phenyl]methanamine hydrochloride | HCID 66969896 | 159.5% |
反応手順
(Step 3) To a solution of 5-chloro-2-(methylsulfonyl)benzonitrile obtained in Step 2 (3.8 g) in ethanol (25 ml) was added an 8N solution of ammonia in methanol (5 ml) and Raney cobalt (19 g, wet). The resulting mixture was stirred overnight at room temperature under a hydrogen atmosphere. The reaction mixture was filtered through celite, and the filtrate was concentrated under reduced pressure. To the residue were added ethanol (10 ml) and a 2 M hydrogen chloride-methanol solution (10 ml). The resulting mixture was concentrated under reduced pressure, and the residual solid was collected by filtration and washed with ethyl acetate to give 1-[5-chloro-2-(methylsulfonyl)phenyl]methanamine hydrochloride (3.6 g) as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07982044B2 |
| 出典データセット | uspto-grants-2011_07 |
| ORD ID | ord-43f5eda27a9a4db4ae668337eac452da |
| 出典メモ | uspto-grants-2011_07 |