反応 #69513

ord-e0b3177f9ddd4c4a82de19eb17756366

反応方程式

CS(=O)(=O)Cl
methanesulfonyl chloride
ClCCl
dichloromethane
COC(C)CCO
3-methoxy-1-butanol
CCN(CC)CC
triethylamine
COC(C)CCOS(C)(=O)=O
3-Methoxybutyl methanesulfonate

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08530504B2uspto-grants-2013_09