반응 #66786

ord-15de7fde64bc4f4184ec232e0020d2d1

용매

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The layers were separated
  2. 2
    workup.ADDITIONthe organic layer was diluted with ethyl acetate
  3. 3
    세척washed with water
  4. 4
    건조The organic layer was dried over sodium sulfate
  5. 5
    기타the solvent was removed in vacuo
  6. 6
    기타The residue was triturated with petroleum ether and tert-butyl methyl ether

실험 절차

To a mixture of pyridin-2-ylmethanol (6.82 g, 62.5 mmol), Aliquat 336 (8.08 g, 20.0 mmol), potassium hydroxide (3.51 g, 62.5 mmol) and water (40 mL) were added toluene (80 mL) and 1,2-dichloro-4-nitrobenzene (10.0 g, 52.1 mmol). The mixture was heated to 60° C. overnight with vigorous stirring. The layers were separated, and the organic layer was diluted with ethyl acetate and washed with water. The organic layer was dried over sodium sulfate, and the solvent was removed in vacuo. The residue was triturated with petroleum ether and tert-butyl methyl ether to yield 6.66 g (48%) of the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08524722B2uspto-grants-2013_09