반응 #65652

ord-bcae0c7a8e3c4c8e905aec27952e2340

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타Evaporate the solvent in vacuo
  2. 2
    workup.ADDITIONdilute with methylene chloride (75 mL)
  3. 3
    세척wash with saturated sodium hydrogen carbonate (35 mL)
  4. 4
    추출Extract the aqueous phase with methylene chloride (30 mL)
  5. 5
    세척wash
  6. 6
    건조dry (Na2SO4)
  7. 7
    기타Evaporate the solvent in vacuo and pass through a plug of silica gel

실험 절차

Dissolve 2-indancarboxylic acid (3.82 g, 23.5 mmol) in methanol (60 mL) and treat with dimethoxypropane (5.8 mL, 47 mmol) and sulfuric acid (0.8 mL). Stir at room temperature for 6 days. Evaporate the solvent in vacuo, dilute with methylene chloride (75 mL) and wash with saturated sodium hydrogen carbonate (35 mL). Extract the aqueous phase with methylene chloride (30 mL), wash combined organics with brine (30 mL) and dry (Na2SO4). Evaporate the solvent in vacuo and pass through a plug of silica gel to give 2-(carbomethoxy)indan as a yellow oil (3.98 g, 96%).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05420271uspto-grants-1995_05