Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Sodium sulfate decahydrate → 1-[3-Chloro-5-(methylsulfanyl)phenyl]methanamine hydrochloride
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Sodium sulfate decahydrate | HCID 62649 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 반응물 | 3-Chloro-5-(methylthio)benzonitrile | HCID 66878686 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 1-[3-Chloro-5-(methylsulfanyl)phenyl]methanamine hydrochloride | HCID 66877840 | 143.4% |
반응 단계
(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).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07985862B2 |
| 출처 데이터셋 | uspto-grants-2011_07 |
| ORD ID | ord-1afe518b5e9346fdaee47126a1c9bd8e |
| 출처 메모 | uspto-grants-2011_07 |