반응 #67284

반응 방정식

5-bromo-3-fluoro-2-[(2R)-oxiran-2-ylmethoxy]phenyl acetate

NaOH

→

crude title compound

[(2S)-7-BROMO-5-FLUORO-2,3-DIHYDRO-1,4-BENZODIOXIN-2-YL]METHANOL

용매

dioxane

반응 조건

후처리

1. 1
   농축concentrated
2. 2
   workup.ADDITIONWater was added
3. 3
   추출the mixture extracted with EtOAc
4. 4
   세척The combined organic phases were washed with brine
5. 5
   건조dried (Na2SO4)
6. 6
   기타evaporated to dryness

실험 절차

1-(5-bromo-3-fluoro-2-[(2R)-oxiran-2-ylmethoxy]phenyl acetate (crude, max 67 mmol) was stirred in dioxane at 0° C. NaOH (15%) was added until the mixture reached pH 14. The mixture was stirred for 30 min at RT and then concentrated. Water was added and the mixture extracted with EtOAc. The combined organic phases were washed with brine, dried (Na2SO4) and evaporated to dryness to give the crude title compound. Yield: 10.3 g. MS m/z (rel. intensity, 70 eV) 262 (M+, bp), 264 (M+, bp), 206 (70), 81 (58), 69 (55), 57 (53).

출처