反応 #473517

ord-e569159be1f043a180086ddbee91d01a

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他equipped with Dean-Stark apparatus over night
  2. 2
    洗浄is washed with aqueous sodium carbonate and water
  3. 3
    その他dried
  4. 4
    その他evaporated to dryness
  5. 5
    その他Purification
  6. 6
    その他Evaporation of the appropriate fractions

実験手順

4-Propyl-cyclohexanecarboxylic acid (10.0 g, 58.0 mmol), 4-bromobutan-1-ol (9.2 g, 60.0 mmol) and a catalytic amount of para-toluene sulphonic acid are stirred under reflux in toluene (300 ml) in a flask equipped with Dean-Stark apparatus over night. The solution is allowed to cool to room temperature, is washed with aqueous sodium carbonate and water, dried and evaporated to dryness. Purification is achieved by flash column chromatography using petrol as eluant. Evaporation of the appropriate fractions gives 4-propyl-cyclohexanecarboxylic acid 4-bromo-butyl ester as the product. The structure is confirmed by 1H NMR spectroscopy and GCMS.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08372307B2uspto-grants-2013_02