반응 #69513

ord-e0b3177f9ddd4c4a82de19eb17756366

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.STIRRINGthe mixture was stirred at room temperature for 30 minutes
  2. 2
    workup.STIRRINGAfter thoroughly shaking the mixture
  3. 3
    기타the organic layer was separated
  4. 4
    세척the organic layer was washed with brine
  5. 5
    건조dried over anhydrous magnesium sulfate
  6. 6
    여과The mixture was then filtered
  7. 7
    workup.DISTILLATIONthe solvent in the filtrate was then distilled off under reduced pressure

실험 절차

To a dichloromethane (30 mL) mixture of 3-methoxy-1-butanol (3.12 g, 30.0 mmol) and triethylamine (4.62 mL, 33.0 mmol), was added methanesulfonyl chloride (4.62 mL, 33.0 mmol) while stirring on ice, and the mixture was stirred at room temperature for 30 minutes. To the mixture, were added water and ethyl acetate. After thoroughly shaking the mixture, the organic layer was separated, and the organic layer was washed with brine and dried over anhydrous magnesium sulfate. The mixture was then filtered, and the solvent in the filtrate was then distilled off under reduced pressure.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08530504B2uspto-grants-2013_09