反応 #4387

ord-4a0ab28d099d4c989edf76e5c61389c1

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the organic layer was separated
  2. 2
    抽出the aqueous layer was extracted with methylene chloride
  3. 3
    洗浄The combined extracts were washed with saturated sodium chloride aqueous solution
  4. 4
    乾燥dried over magnesium sulfate
  5. 5
    その他evaporated in vacuo
  6. 6
    その他The crystalline residue was recrystallized from ethyl acetate

実験手順

To a mixture of 2-amino-3-hydroxypyridine (7 g) and Adogen 464 (Trademark: prepared by Aldrich Chemical Co.) (0.4 g) in 40% aqueous sodium hydroxide (32 ml) and methylene chloride (32 ml) was added 2-methylbenzyl chloride (8.42 ml) at ambient temperature. After being stirred for 24 hours, the organic layer was separated and the aqueous layer was extracted with methylene chloride. The combined extracts were washed with saturated sodium chloride aqueous solution, dried over magnesium sulfate, and evaporated in vacuo. The crystalline residue was recrystallized from ethyl acetate to give 2-amino-3-(2-methylbenzyloxy)pyridine (7.56 g).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04725601uspto-grants-1988_02