反応 #348651

ord-99c662b7e86b41ef9d75ebd3247127d6

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過filtered
  2. 2
    濃縮concentrated to dryness
  3. 3
    その他leaving a white solid
  4. 4
    ろ過the solution filtered through celite
  5. 5
    濃縮concentrated again
  6. 6
    その他providing a white solid, which upon trituration with ether

実験手順

A solution of 5.3 g of 2,3-dihydro-1'-benzylspiro[benzofuran-2,4'-piperidine], free base of B, in 250 ml of isopropyl alcohol is hydrogenated with a Paar shaker, 50 psig, 65°-70° C. and 1 g of a 10% palladium/carbon catalyst until the uptake of hydrogen is completed. Thereafter, the solution is successively permitted to cool to ambient temperature, filtered and concentrated to dryness, leaving a white solid. The solid is dissolved in a benzene-ether mixture, the solution filtered through celite and then concentrated again providing a white solid, which upon trituration with ether, provides the product, 2,3-dihydrospiro[benzofuran-2,4'-piperidine], mp 56°-58.5° C.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04166120uspto-grants-1979_08