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Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 715493생성일: 2026년 10월 27일

Dichloromethane → 3-({[(2R,3R,7S)-2,3-diphenyl-1,4-dioxaspiro[4.5]dec-7-yl]methyl}amino)-4-nitrobenzonitrile

https://huagongshe.com/reaction/715493

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참여 물질

역할이름HCID투입량
반응물DichloromethaneHCID 6344—
반응물Potassium CarbonateHCID 11430—
반응물3-Fluoro-4-nitrobenzonitrileHCID 2783399—
반응물1-[(2R,3R,7S)-2,3-diphenyl-1,4-dioxaspiro[4.5]dec-7-yl]methanamineHCID 71116053—
용매MethanolHCID 887—
용매AcetonitrileHCID 6342—
생성물3-({[(2R,3R,7S)-2,3-diphenyl-1,4-dioxaspiro[4.5]dec-7-yl]methyl}amino)-4-nitrobenzonitrileHCID 7111620988%

반응 단계

A mixture of 3-fluoro-4-nitrobenzonitrile (55.5 g, 334 mmol), 1-[(2R,3R,7S)-2,3-diphenyl-1,4-dioxaspiro[4.5]dec-7-yl]methanamine (103 g, 318 mmol) and potassium carbonate (88 g, 637 mmol) in acetonitrile (2654 mL) was stirred at RT for 5 days (˜200 mL DCM was added to help with solubility). The resulting solution was filtered and the solids washed with MeCN. The resulting solution was concentrated to give the crude product that was dissolved in MeOH (500 mL) and allowed to crystallize with stirring. The slurry was allowed to stir at RT overnight, filtered and the solids dried under reduced pressure to give 3-({[(2R,3R,7S)-2,3-diphenyl-1,4-dioxaspiro[4.5]dec-7-yl]methyl}amino)-4-nitrobenzonitrile (131.41 g, 88% yield). The product was used without further purification.

출처 및 근거

DOI10.6084/m9.figshare.5104873.v1
특허 번호US09187464B2
출처 데이터셋uspto-grants-2015_11
ORD IDord-487b7f2e91fd435589bbee19d4572d21
출처 메모uspto-grants-2015_11