反応 #2981

ord-930d75a478a44c1f993455a3cf0bd573

反応方程式

CCN(CC)CC
triethylamine
CS(=O)(=O)Cl
mesyl chloride
COc1ccc2cccc(CCO)c2c1
2-(7-methoxy-1-naphthyl)ethanol
COc1ccc2cccc(CCOS(C)(=O)=O)c2c1
2-(7-METHOXY-1-NAPHTHYL)ETHYL MESYLATE

反応条件

温度
-10°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.WAITThe mixture is left
  2. 2
    workup.STIRRINGstirring for 30 minutes
  3. 3
    抽出The aqueous phase is extracted with 3 times 50 cm3 of dichloromethane
  4. 4
    洗浄the organic phase is washed with 3 times 20 cm3 of 1N hydrochloric acid solution
  5. 5
    乾燥with water, dried over potassium carbonate
  6. 6
    その他evaporated
  7. 7
    その他The oily residue is recrystallized

実験手順

In a 250-cm3 flask, 4 g of 2-(7-methoxy-1-naphthyl)ethanol are dissolved in 100 cm3 of dichloromethane, and 3.3 cm3 of triethylamine are added. The mixture is cooled in an ice bath at -10° C. and 2.75 g of mesyl chloride are then added dropwise and with stirring. The mixture is left stirring for 30 minutes. The aqueous phase is extracted with 3 times 50 cm3 of dichloromethane, and the organic phase is washed with 3 times 20 cm3 of 1N hydrochloric acid solution and then with water, dried over potassium carbonate and evaporated. The oily residue is recrystallized.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05731352uspto-grants-1998_03