참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 4-Fluorobenzaldehyde | HCID 68023 | — |
| 반응물 | (2-Carboxyethyl)triphenylphosphonium chloride | HCID 10270534 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 반응물 | HCID 178418361 | HCID 178418361 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-(4-Fluorophenyl)but-3-enoic acid | HCID 10397385 | 50% |
반응 단계
74.4 g of 4-fluorobenzaldehyde and 233.6 g of β-carboxyethyl-triphenyl phosphonium chloride were suspended in 700 ml of tetrahydrofuran and these were incubated on ice and stirred. Into this 500 ml tetrahydrofuran solution of 141.4 g of potassium tert-butoxide was added slowly dropwise. 30 minutes after temperature was brought to room temperature and then they were stirred for 10 hours. After adding thereto ice water and cleaning with ether, the hydrogen-ion concentration of water layer was set to pH2 with undiluted hydrochloric acid. Extraction was then made with ethyl acetate. After drying with magnesium sulfate and concentration made under reduced pressure, the solid obtained was recrystallized from hydrous ethanol, and 53.98 g of marked compound (yield: 50%) was obtained as white needle crystal.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US05607953 |
|---|
| 출처 데이터셋 | uspto-grants-1997_03 |
|---|
| ORD ID | ord-1ed36f677c7944f586fef193ca317de3 |
|---|
| 출처 메모 | uspto-grants-1997_03 |
|---|
