反应详情

Potassium tert-butoxide (7.53 g) was added to a solution 2-chloro-4-bromoacetophenone (CAS Reg. No. 252561-81-2, 10.45 g) and (methoxymethyl)-triphenylphosphosium chloride (21.48 g) in THF (100 ml) at room temperature. The mixture was stirred for 1 h at room temperature. 25% aqueous HCl (90 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 1:4) to give the title compound (8.1 g) as a yellow oil. MS (m/e, ISP neg. ion)=247.2 [M−H+].

1. customat room temperature
2. stirringThe resulting mixture was stirred 1 h at room temperature
3. additionpoured
4. extractionAfter neutralization, the mixture was extracted with EtOAc
5. dry with materialThe combined organic layers were dried over Na2SO4
6. concentrationconcentrated to an oil
7. customThe residue was purified by flash chromatography (SiO2, EtOAc/heptane 1:4)