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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

반응식

참여 물질

역할이름HCID투입량
반응물Dimethyl DisulfideHCID 12232—
반응물(5-Bromo-2-triisopropylsilanyl-2,7,8,9-tetrahydro-6-oxa-2-azabenzo[cd]azulen-8-yl)dimethylamineHCID 69736345—
반응물ButyllithiumHCID 178418339—
용매TetrahydrofuranHCID 8028—
용매Ammonium ChlorideHCID 25517—
생성물Dimethyl-(5-methylsulfanyl-2-triisopropylsilanyl-2,7,8,9-tetrahydro-6-oxa-2-azabenzo[cd]-azulen-8-yl)amineHCID 6973643369%

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

DOI10.6084/m9.figshare.5104873.v1
특허 번호US06858640B2
출처 데이터셋uspto-grants-2005_02
ORD IDord-88856aa7067d48b783d67b38e16f531d
출처 메모uspto-grants-2005_02