반응 #64813

ord-198b9a41cec24196b85b029ecdae8852

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타After recooling to 0° C.
  2. 2
    workup.STIRRINGthe thick white suspension was stirred briskly for about 30 minutes
  3. 3
    여과The suspension was filtered through silica gel
  4. 4
    세척the filter cake was washed thoroughly with ethyl ether
  5. 5
    농축The filtrate was concentrated
  6. 6
    기타dried under high vacuum
  7. 7
    기타to afford 4.15 g

실험 절차

Benzofuran-2-carboxylic acid (4.59 g., 28.3 mmol) as a solution in dry ethyl ether (100 mL) was added dropwise over 15 minutes to a suspension of lithium aluminum hydride (4.3 g., 113 mmol) in ethyl ether (180 mL) at 0° C. The reaction mixture was stirred for 2 hours while warming to room temperature. After recooling to 0° C., 4.3 mL of water was added with extreme caution. Sodium hydroxide (4.3 mL, 15% in water) was then added followed by an additional 12.9 mL of water. Magnesium sulfate (about 10 g.) was added and the thick white suspension was stirred briskly for about 30 minutes. The suspension was filtered through silica gel and the filter cake was washed thoroughly with ethyl ether. The filtrate was concentrated and dried under high vacuum to afford 4.15 g. of the title A product as a light yellow oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05414017uspto-grants-1995_05