Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethyl phosphonoacetate → Ethyl 3-(2,3,4-trimethoxyphenyl)prop-2-enoate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethyl phosphonoacetate | HCID 13345 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2,3,4-Trimethoxybenzaldehyde | HCID 75006 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | Ethyl 3-(2,3,4-trimethoxyphenyl)prop-2-enoate | HCID 67200008 | — |
반응 단계
Sodium hydride (60% dispersion in mineral oil; 245 mg) was suspended in THF (1 mL) under an argon atmosphere, to the suspension ethyl diethylphosphonoacetate (1.11 mL) was added dropwise under ice cooling, and the mixture was stirred for 30 minutes. After 2,3,4-trimethoxybenzaldehyde (1.0 g) was then added to the mixture, the reaction mixture was stirred at room temperature for 30 minutes and concentrated under reduced pressure. The residue was dissolved in chloroform, and the solution was washed with water and saturated brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=1:1) to obtain the title compound.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06552188B2 |
| 출처 데이터셋 | uspto-grants-2003_04 |
| ORD ID | ord-ad0405e069a04048add29f64914eab36 |
| 출처 메모 | uspto-grants-2003_04 |