反応 #51274

ord-fb17e6201ae24177862d7baad47c5a19

溶媒

反応条件

温度
7.5°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The solution obtained
  2. 2
    workup.STIRRINGthe reaction mixture is stirred for one hour at room temperature
  3. 3
    抽出extracted with ethyl ether
  4. 4
    その他the organic phase is separated
  5. 5
    乾燥dried over magnesium sulphate
  6. 6
    その他evaporated
  7. 7
    その他46.00 g (130%) of the expected compound are collected in the form of an orange oil

実験手順

40.00 g (140.2 mmol) of 2,4-di-tert-butyl-6-bromophenol and 400 ml of DMF are introduced into a one liter three-necked flask. The solution obtained is cooled to 5-10° C., 4.70 g of sodium hydride are added and the mixture is stirred at 10° C. for 30 minutes. 11.7 ml (154.0 mmol) of chloromethyl methyl ether are then added dropwise and the reaction mixture is stirred for one hour at room temperature. The reaction mixture is poured into a 1N HCl/ethyl ether mixture and extracted with ethyl ether and the organic phase is separated by settling, dried over magnesium sulphate and evaporated. 46.00 g (130%) of the expected compound are collected in the form of an orange oil.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06849658B2uspto-grants-2005_02