Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 4-[3-Chloro-4-(1-methyl-2-oxo-ethyl)-phenoxy]-benzonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Methoxymethyl-triphenylphosphonium chloride | HCID 2723798 | — |
| 반응물 | Potassium tert-butoxide | HCID 23665647 | — |
| 반응물 | 4-(4-Acetyl-3-chlorophenoxy)benzonitrile | HCID 64335501 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 4-[3-Chloro-4-(1-methyl-2-oxo-ethyl)-phenoxy]-benzonitrile | HCID 86645948 | — |
반응 단계
Potassium tert-butoxide (248 mg) was added to a solution 4-(4-acetyl-3-chloro-phenoxy)-benzonitrile (500 mg) and (methoxymethyl)-triphenylphosphonium chloride (694 mg) in THF (10 ml) at room temperature. The mixture was stirred for 1 h at room temperature. 25% aqueous HCl (4 ml) was added. The resulting mixture was stirred 1 h at room temperature and poured then carefully to a saturated aqueous NaHCO3 solution. After neutralization, the mixture was extracted with EtOAc. The combined organic layers were dried over Na2SO4 and then concentrated to an oil. The residue was purified by flash chromatography (SiO2, EtOAc/heptane 1:2) to give the title compound (450 mg) as yellow oil. MS (m/e, ISP neg. ion)=284.3 [M−H+].
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08138189B2 |
| 출처 데이터셋 | uspto-grants-2012_03 |
| ORD ID | ord-e8ddd91e87ed4d8bb16d6688a903ae58 |
| 출처 메모 | uspto-grants-2012_03 |