반응 #44015

ord-71b99c62f1f846faa023e22183d00378

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척Organic layer was washed with 0.2 N citric acid, water, brine
  2. 2
    건조dried over anhydrous Na2SO4
  3. 3
    여과The solution was filtered
  4. 4
    기타evaporated
  5. 5
    기타The residue was purified by flash chromatography
  6. 6
    세척eluting with EtOAc-hexane (1:3) mixture

실험 절차

The crude cis-2,6-dimethylpiperidin-4-one 91 from previous experiment (1.1 g, 8.6 mmol) was dissolved in CH2Cl2 (50 mL) and triethylamine (5 mL, 35 mmol) was added. Stirred solution was treated with 4-chlorobenzenesulfonyl chloride (2.2 g, 9.5 mmol). The mixture was stirred for 24 hr then was divided between water (100 mL) and CH2Cl2 (100 mL). Organic layer was washed with 0.2 N citric acid, water, brine and dried over anhydrous Na2SO4. The solution was filtered and evaporated. The residue was purified by flash chromatography, eluting with EtOAc-hexane (1:3) mixture. Yield 60 mg (2% after two steps).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07732609B2uspto-grants-2010_06