Benzaldehyde → 3-Methyl-1-phenyl-1buten-1ol

HRID 984509

反応式

HRID 984509 の反応式
[CH:1](=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:9][C:10](=[CH2:14])[CH2:11][Mg]Cl.[NH4+].[Cl-]>C1COCC1>[CH3:9][CH:10]([CH3:14])[CH:11]=[C:1]([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)[OH:8]

参加物

5

実験手順

To a solution of benzaldehyde (3.05 mL, 30 mmol) in THF (30 mL) was added 2-methylallylmagnesium chloride (0.8 M in THF, 45 mL, 36 mmol, 1.2 equiv) under N2 at 0° C. (internal). The mixture was warmed to room temperature and was stirred for 1.5 h. The mixture was then poured into saturated aqueous NH4Cl solution (30 mL) and was extracted with EtOAc (2×30 mL). The combined organic layers were washed with brine (30 mL), then were dried (Na2SO4) and filtered. The solvent was removed by rotary evaporation and the residue was purified by Kugelrohr distillation to afford 4.33 g (89%) of 3-methyl-1-phenyl-1buten-1-ol as a colorless oil.

後処理

  1. extractionwas extracted with EtOAc (2×30 mL)
  2. washThe combined organic layers were washed with brine (30 mL)
  3. dry with materialwere dried (Na2SO4)
  4. filtrationfiltered
  5. customThe solvent was removed by rotary evaporation
  6. distillationthe residue was purified by Kugelrohr distillation

出典と根拠

ORDレコード
ord-ff8f1e4b896a40698672aa28560c941d
出典データセット
uspto-grants-2005_03
特許番号
US06867323B2

関連ノート

読み込み中…