反応 #1596945

ord-609d76306b6f4c51aa02b2d46b205656

反応方程式

CCCC1COC(c2ccc(OCc3ccccc3)c(F)c2)CC1Br
2-(4-benzyloxy-3-fluorophenyl)-4-bromo-5-propyltetrahydropyran
CCN(CC)CC
triethylamine
CCCC1CCC(c2ccc(O)c(F)c2)OC1
2-fluoro-4-(5-propyltetrahydropyran-2-yl)phenol

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他the organic phase is separated off
  2. 2
    抽出The aqueous phase is extracted with MTBE
  3. 3
    洗浄The combined organic phases are washed with water
  4. 4
    その他dried
  5. 5
    濃縮The solution is concentrated to dryness
  6. 6
    その他the residue is used directly for the following reaction

実験手順

123.0 g (0.30 mol) of 2-(4-benzyloxy-3-fluorophenyl)-4-bromo-5-propyltetrahydropyran are hydrogenated in toluene/water in the presence of Pd/C (5% of Pd) and 86.0 ml (0.60 mol) of triethylamine. The reaction solution is diluted with MTBE, and the organic phase is separated off. The aqueous phase is extracted with MTBE. The combined organic phases are washed with water and dried using sodium sulfate. The solution is concentrated to dryness, and the residue is used directly for the following reaction.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08211513B2uspto-grants-2012_07