Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Fluoride → 1-(3,4-Dimethoxyphenyl)-2-nitro-6-cyano-6-(prop-2-yl)-6-(3,4-dimethoxyphenyl)hexan-3-ol
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Fluoride | HCID 522689 | — |
| 반응물 | 3-(3,4-Dimethoxyphenyl)-2-methyl-6-oxohexane-3-carbonitrile | HCID 3015370 | — |
| 반응물 | Benzene, 1,2-dimethoxy-4-(2-nitroethyl)- | HCID 10036050 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 생성물 | 1-(3,4-Dimethoxyphenyl)-2-nitro-6-cyano-6-(prop-2-yl)-6-(3,4-dimethoxyphenyl)hexan-3-ol | HCID 13745754 | 73.9% |
반응 단계
A mixture of 2-(3,4-dimethoxyphenyl)-1-nitroethane (4, 135 g, 0.64 mol), 2-(3,4-dimethoxyphenyl)-2-(3-oxopropyl)-2-isopropylacetonitrile (7, 156 g, 0.57 mol) and KF (19.3 g, anhydrous, Aldrich) in 2-propanol (2.0 L) was heated to 50°-55° C. for about 40 hours. The mixture was then cooled to room temperature and the isopropanol removed in vacuo. The residue was dissolved in CH2Cl2 (1.6 L) and filtered through Celite (50 g). The filtrate was extracted with saturated aqueous NaHCO3 (2×500 mL), the organic layer evaporated, and the product recrystallized from ethyl acetate-hexane (1:1) to yield 1-(3,4-dimethoxyphenyl)-2-nitro-6-cyano-6-(i-propyl)-6-(3,4-dimethoxyphenyl)-hexan-3-ol (8, 205 g, m.p. 171°-173° C., MS m/e 486(M+)).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04613606 |
| 출처 데이터셋 | uspto-grants-1986_09 |
| ORD ID | ord-92b6f07b7f574e82a63201563d3f281b |
| 출처 메모 | uspto-grants-1986_09 |