Sodium Carbonate → 3-[4-[1-Hydroxyimino-2-(2-fluorophenyl)ethyl]piperidino]methyl-1H-pyrazin-2-one

HRID 914889노트

반응식

HRID 914889 반응식
[F:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH2:8][C:9]([CH:11]1[CH2:16][CH2:15][N:14]([CH2:17][C:18]2[C:19](=[O:24])[NH:20][CH:21]=[CH:22][N:23]=2)[CH2:13][CH2:12]1)=O.Cl.[NH2:26][OH:27].C(=O)([O-])[O-].[Na+].[Na+].[Cl-].[NH4+]>C(O)C.ClCCl.O>[OH:27][N:26]=[C:9]([CH:11]1[CH2:16][CH2:15][N:14]([CH2:17][C:18]2[C:19](=[O:24])[NH:20][CH:21]=[CH:22][N:23]=2)[CH2:13][CH2:12]1)[CH2:8][C:3]1[CH:4]=[CH:5][CH:6]=[CH:7][C:2]=1[F:1]

참가 물질

8

반응물 4

HCID 10340Sodium CarbonateHCID 25517Ammonium ChlorideHCID 443297Hydroxyamine hydrochlorideHCID 101933903-[4-[2-(2-Fluorophenyl)acetyl]piperidino]methyl-1H-pyrazin-2-one

생성물 1

HCID 866013883-[4-[1-Hydroxyimino-2-(2-fluorophenyl)ethyl]piperidino]methyl-1H-pyrazin-2-one수율 70%

시약·촉매·용매 3

HCID 702Ethanol용매HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

After suspending 150 mg of 3-[4-[2-(2-fluorophenyl)acetyl]piperidino]methyl-1H-pyrazin-2-one in 3 ml of ethanol, 47 mg of hydroxylamine hydrochloride and 193 mg of sodium carbonate were added while stirring and the mixture was heated to reflux for 1 hour. Water and saturated aqueous ammonium chloride solution were added to the reaction solution for adjustment to pH 7, and extraction was performed with dichloromethane. The organic layer was washed with brine and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. Diethyl ether was added and the insoluble portion was filtered out to obtain the title compound (109 mg, 70% yield).

후처리

  1. additionwere added
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 1 hour
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. additionDiethyl ether was added
  8. filtrationthe insoluble portion was filtered out

출처 및 근거

ORD 기록
ord-a833c530fa07482f9e83b5e5c1a6c342
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265108B2

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