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
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 3-Fluoro-4-nitrobenzonitrile | HCID 2783399 | — |
| 반응물 | 1-[(2R,3R,7S)-2,3-diphenyl-1,4-dioxaspiro[4.5]dec-7-yl]methanamine | HCID 71116053 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 3-({[(2R,3R,7S)-2,3-diphenyl-1,4-dioxaspiro[4.5]dec-7-yl]methyl}amino)-4-nitrobenzonitrile | HCID 71116209 | 88% |
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
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US09187464B2 |
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| 출처 데이터셋 | uspto-grants-2015_11 |
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| ORD ID | ord-487b7f2e91fd435589bbee19d4572d21 |
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| 출처 메모 | uspto-grants-2015_11 |
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