Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 25338생성일: 2026년 10월 23일
Dimethyl Disulfide → Dimethyl-(5-methylsulfanyl-2-triisopropylsilanyl-2,7,8,9-tetrahydro-6-oxa-2-azabenzo[cd]-azulen-8-yl)amine
https://huagongshe.com/ko/reaction/25338
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dimethyl Disulfide | HCID 12232 | — |
| 반응물 | (5-Bromo-2-triisopropylsilanyl-2,7,8,9-tetrahydro-6-oxa-2-azabenzo[cd]azulen-8-yl)dimethylamine | HCID 69736345 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 용매 | Ammonium Chloride | HCID 25517 | — |
| 생성물 | Dimethyl-(5-methylsulfanyl-2-triisopropylsilanyl-2,7,8,9-tetrahydro-6-oxa-2-azabenzo[cd]-azulen-8-yl)amine | HCID 69736433 | 69% |
반응 단계
A solution of compound (42) 451 mg in dry tetrahydrofuran 5 ml was cooled at −70° C. n-BuLi (1.56 mol/l hexane solution) 1.3 ml was added dropwise to the solution and the mixture was stirred for 1 h. Then, dimethyldisulfide 185 μl was added and the mixture was stirred for 2 h. The reaction mixtures was diluted with an aqueous ammonium chloride solution and extracted with ethyl acetate. The extracts were washed with brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue obtained was chromatographed on aluminum oxide in ethyl acetate:hexane (1:5) to give the titled compound as colorless crystals, 289.8 mg. Yield 69%. This was recrystallized from hexane to give the titled compound as colorless crystals, m.p. 77-79° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06858640B2 |
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| 출처 데이터셋 | uspto-grants-2005_02 |
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| ORD ID | ord-88856aa7067d48b783d67b38e16f531d |
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| 출처 메모 | uspto-grants-2005_02 |
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