반응 #60386

ord-30652c6c4f424175b90fd002eef49a3c

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The solvent was evaporated in vacuo
  2. 2
    기타The residue was purified by silica gel chromatography (3%-5% MeOH—CH2Cl2)

실험 절차

To a mixture of 6-hydroxy-1-tetralone (Aldrich, 1.0 g, 6.17 mmol, 1.0 eq), N,N-dimethylethanolamine (Aldrich, 0.93 mL, 9.26 mmol, 1.5 eq), and triphenylphosphine (Aldrich, 2.43 g, 9.26 mmol, 1.5 eq) in THF (10 mL) was added diethyl azodicarboxylate (Aldrich, 1.94 mL, 12.34 mmol, 2.0 eq) at 0° C. The reaction mixture was gradually warmed to RT and continued to stir overnight. The solvent was evaporated in vacuo. The residue was purified by silica gel chromatography (3%-5% MeOH—CH2Cl2) to provide the product as orange oil. MS (ESI): 234 (M+H)+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07425631B2uspto-grants-2008_09