反応 #530841

ord-587585ab1af74487abede341db9deaa5

反応条件

温度
225°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他fitted with a water trap
  2. 2
    workup.DISSOLUTIONdissolved
  3. 3
    温度to cool
  4. 4
    workup.ADDITIONthe base was neutralized by the addition of 5 ml
  5. 5
    その他Sodium chloride from neutralization of the base was removed by filtration
  6. 6
    workup.DISTILLATIONthe filtrate was distilled under vacuum

実験手順

To 1.15 grams of metallic sodium (0.05 moles) was added to 59 grams of 1,6-hexanediol (0.5 moles) in a 250 ml flask fitted with a water trap and the mixture was stirred until the sodium dissolved. There was then added 20.6 grams of 2,6-di-tert.-butylphenol (0.1 mole) and the mixture was heated for 7.5 hours at 225° C. The mixture was allowed to cool and the base was neutralized by the addition of 5 ml. of concentrated hydrochloric acid. Sodium chloride from neutralization of the base was removed by filtration and the filtrate was distilled under vacuum. There was obtained 20.4 grams (66.6% yield) of 6-(3,5-di-tert.-butyl-4-hydroxyphenyl)hexanol.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04260832uspto-grants-1981_04