반응 #340363

ord-1999b5c21a8746d19205e84693954fdc

용매

반응 조건

온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도cooled to 15° C.
  2. 2
    기타quenched by cautious addition of water (0.15 mL)
  3. 3
    여과filtered
  4. 4
    세척washed with THF (3×5 mL)
  5. 5
    농축The filtrate was concentrated in vacuo

실험 절차

To a solution of the lactam from Example 22C (0.46 g) in THF (5 mL) was added 1M LiAlH4 (4.0 mL). The mixture was heated at 50° C. for 2 h, cooled to 15° C., and quenched by cautious addition of water (0.15 mL), followed by 15% NaOH (0.15 mL), then water (0.456 mL). The mixture was stirred for 5 minutes and filtered and washed with THF (3×5 mL). The filtrate was concentrated in vacuo to afford 442 mg of the title compound as a clear oil (quantitative yield). MS (CI) m/z 217 (M+H)+; 1H NMR: δ 1.8-1.5 (m, 3H), 2.33-2.10 (m, 2H), 2.8-2.4 (m, 8H), 3.75 (s, 2H), 7.25 ppm (m, 5H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07872010B2uspto-grants-2011_01