반응 #69263

ord-5c426494f53b403092b47b43b4284363

반응 조건

온도
0°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타The reaction was then quenched with water and 1 N NaOH (0.5 mL of each) and
  2. 2
    여과then filtered
  3. 3
    세척The filtered solid was washed with ether
  4. 4
    농축the combined ether filtrate was concentrated
  5. 5
    기타a rotary evaporator
  6. 6
    기타to give the product

실험 절차

1,4-Dioxa-spiro[4.5]decan-8-one (2.00 g, 0.0128 mol) was dissolved in ether (50 mL) and the mixture was cooled to 0° C. To the reaction was added 1 M lithium tetrahydroaluminate in ether (7.0 mL) and this mixture was stirred at 0° C. for 2 hours at which time TLC analysis showed no starting material present. The reaction was then quenched with water and 1 N NaOH (0.5 mL of each) and then filtered. The filtered solid was washed with ether and the combined ether filtrate was concentrated using a rotary evaporator to give the product. NMR (CDCl3): 3.94 (m, 4H), 3.81 (m, 1H), 1.79-1.92 (m, 4H), 1.54-1.70 (m, 4H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08530485B2uspto-grants-2013_09