HRID396317

反应详情

EQUATION

反应方程式

HRID 396317 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1-benzylpiperidin-4-one (10 g, 53.0 mmole) was added to the stirred suspension of potassium tert. butoxide (6.0 g, 54.0 mmole) in tetrahydrofuran (50 ml) at 10° C. The reaction mixture was stirred for 15 min, isopropyl iodide (10 g, 54.0 mmole) was added at 10° C. The resulting mixture allowed coming at room temperature and stirred for 16 hr, refluxed for 3 hr and concentrated to dryness. The residue was triturated with water, extracted with ethyl acetate, dried (Na2SO4) and concentrated to give crude product, which was purified through column chromatography. Elute from 10% ethyl acetate in hexane afforded 1-benzyl-3-isopropylpiperid-4-one. Yield 3.3 g (28%), C15H21NO, m/z 232 (M+1).

WORKUP

后处理

  1. customallowed coming at room temperature
  2. stirringstirred for 16 hr
  3. temperaturerefluxed for 3 hr
  4. concentrationconcentrated to dryness
  5. customThe residue was triturated with water
  6. extractionextracted with ethyl acetate
  7. dry with materialdried (Na2SO4)
  8. concentrationconcentrated
  9. customto give crude product, which
  10. customwas purified through column chromatography
  11. washElute from 10% ethyl acetate in hexane