반응 #340363
ord-1999b5c21a8746d19205e84693954fdc
반응 방정식
용매
반응 조건
온도
50°CELSIUS
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도cooled to 15° C.
- 2기타quenched by cautious addition of water (0.15 mL)
- 3여과filtered
- 4세척washed with THF (3×5 mL)
- 5농축The 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).