반응 #2184651

ord-63440056bbb84706876a04bf8c1daad5

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter completion of the addition
  2. 2
    기타After completion of the reaction
  3. 3
    추출extracted with toluene
  4. 4
    기타The organic layer after separation
  5. 5
    세척was washed with a saturated aqueous solution of sodium chloride
  6. 6
    건조dried over anhydrous magnesium sulfate
  7. 7
    농축concentrated under reduced pressure

실험 절차

To 300 ml of dehydrated dichloromethane solution containing 60.0 g (247 mmol) of 4-bromo-2-cyclopropoxy-1-methoxybenzene obtained in Reference Example 7-(c) was added 300 ml of dichloromethane solution containing 1M boron tribromide under argon atmosphere at −70° C. After completion of the addition, the mixture was gradually raised to 0° C., and stirred at the same temperature for 30 minutes. After completion of the reaction, the reaction mixture was poured into ice-water, and extracted with toluene. The organic layer after separation was washed with a saturated aqueous solution of sodium chloride, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to obtain 58.6 g of the title compound as a blue-greenish solid substantially quantitatively.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08450319B2uspto-grants-2013_05