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Sodium sulfate decahydrate → 1-[3-Chloro-5-(methylsulfanyl)phenyl]methanamine hydrochloride
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium sulfate decahydrate | HCID 62649 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | 3-Chloro-5-(methylthio)benzonitrile | HCID 66878686 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-[3-Chloro-5-(methylsulfanyl)phenyl]methanamine hydrochloride | HCID 66877840 | 143.4% |
反応手順
(Step 2) To a suspension of lithium aluminum hydride (0.79 g) in tetrahydrofuran (200 ml) was added 3-chloro-5-(methylsulfanyl)benzonitrile obtained in Step 1 (3.2 g) at 0° C. The mixture was stirred at room temperature for 3 hr, and treated with sodium sulfate 10 hydrate. The mixture was stirred at room temperature for 30 min, and the inorganic substance was filtered off through celite. The filtrate was concentrated under reduced pressure. The residue was dissolved in methanol, and 4N hydrogen chloride-ethyl acetate solution (5 ml) was added. The mixture was crystallized from methanol-ethyl acetate, and the obtained crystals were washed with ethyl acetate to give 1-[3-chloro-5-(methylsulfanyl)phenyl]methanamine hydrochloride (2.8 g).
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-e2751b74a1d1420681dfe601e99120eb |
| 出典メモ | uspto-grants-2011_07 |