反应 #543575

ord-c01aed61e13749cf93cc2d4a7e8b5f3b

反应方程式

ClCc1ccc(Cl)cc1
4-chlorobenzyl chloride
CCN(CC)CC
triethylamine
CN(C)C=O
DMF
O=C1CCN(Cc2ccc(Cl)cc2)CC1
subtitled compound
O=C1CCN(Cc2ccc(Cl)cc2)CC1
1-(4-Chlorobenzyl)-4-piperidinone

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The volatiles were removed in vacuo, residue
  2. 2
    workup.DISSOLUTIONwas dissolved in ethylacetate
  3. 3
    洗涤washed with water (H2O), organic layer
  4. 4
    干燥was dried over sodium sulphate (Na2SO4)
  5. 5
    过滤filtered
  6. 6
    浓缩concentrated
  7. 7
    其他The residue was purified by silica gel flash chromatography

实验过程

To a solution of 4-piperidine trifluoroacetate obtained from step (iv) (853 mg, 4.0 mmol) in DMF was added triethylamine (2.66 mL, 19.2 mmol), followed by 4-chlorobenzyl chloride (753 mg, 4.8 mmol) and the reaction mixture was stirred overnight at room temperature. The volatiles were removed in vacuo, residue was dissolved in ethylacetate, washed with water (H2O), organic layer was dried over sodium sulphate (Na2SO4), filtered and concentrated. The residue was purified by silica gel flash chromatography to give the subtitled compound (350 mg).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07186718B2uspto-grants-2007_03