Ammonium cerium (IV) nitrate → HCID 66608280, 화합물

HRID 71208

반응식

HRID 71208 반응식
COC1C=CC(C[N:8]2[CH2:13][CH2:12][CH2:11][C:10]([CH3:24])([O:14][C:15]3[CH:20]=[C:19]([F:21])[C:18]([F:22])=[C:17]([F:23])[CH:16]=3)[C:9]2=[O:25])=CC=1.[N+]([O-])([O-])=O.[NH4+].[Ce+4].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.[N+]([O-])([O-])=O>C(#N)C.O.C(OCC)(=O)C.C(=O)([O-])O.[Na+]>[CH3:24][C:10]1([O:14][C:15]2[CH:20]=[C:19]([F:21])[C:18]([F:22])=[C:17]([F:23])[CH:16]=2)[CH2:11][CH2:12][CH2:13][NH:8][C:9]1=[O:25]

참가 물질

7

반응물 2

HCID 9869224Ammonium cerium (IV) nitrate2회HCID 666083191-(4-Methoxybenzyl)-3-methyl-3-(3,4,5-trifluorophenoxy)piperidin-2-one

생성물 1

HCID 66608280HCID 66608280, 화합물수율 57.8%

시약·촉매·용매 4

HCID 962Water용매HCID 6342Acetonitrile용매HCID 8857Ethyl Acetate용매HCID 516892Sodium Bicarbonate용매

실험 절차

To a mixture of 1-(4-methoxybenzyl)-3-methyl-3-(3,4,5-trifluorophenoxy)piperidin-2-one (76.2 mg) in acetonitrile (1 mL) was added a mixture of cerium(IV) ammonium nitrate (275 mg) in water (1 mL) at room temperature, and the mixture was stirred overnight. Cerium(IV) ammonium nitrate (110 mg) was added, and the mixture was stirred at room temperature for 1 hr. The reaction mixture was diluted with ethyl acetate and saturated aqueous sodium hydrogen carbonate solution, and the insoluble material was removed by filtration. The organic layer was separated, washed with water and saturated brine, and dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (NH, ethyl acetate) and silica gel column chromatography (ethyl acetate/hexane) to give the title compound (30.1 mg).

후처리

  1. additionwas added
  2. stirringthe mixture was stirred at room temperature for 1 hr
  3. customthe insoluble material was removed by filtration
  4. customThe organic layer was separated
  5. washwashed with water and saturated brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. customthe solvent was evaporated under reduced pressure
  8. customThe residue was purified by silica gel column chromatography (NH, ethyl acetate) and silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-61f80022f8fe4e3a9ca67e2e0be6b69b
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822699B2

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