Water → 6-[2-[4-(2-Fluorophenoxymethyl)piperidino]ethyl]-1-methyl-1H-pyrazin-2-one

HRID 890104노트

반응식

HRID 890104 반응식
[F:1][C:2]1[CH:24]=[CH:23][CH:22]=[CH:21][C:3]=1[O:4][CH2:5][CH:6]1[CH2:11][CH2:10][N:9]([CH2:12][CH2:13][C:14]2[NH:19][C:18](=[O:20])[CH:17]=[N:16][CH:15]=2)[CH2:8][CH2:7]1.[H-].[Na+].[CH3:27]I.O>CN(C)C=O.C(OCC)(=O)C>[F:1][C:2]1[CH:24]=[CH:23][CH:22]=[CH:21][C:3]=1[O:4][CH2:5][CH:6]1[CH2:7][CH2:8][N:9]([CH2:12][CH2:13][C:14]2[N:19]([CH3:27])[C:18](=[O:20])[CH:17]=[N:16][CH:15]=2)[CH2:10][CH2:11]1

참가 물질

7

반응물 4

HCID 962WaterHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 97976346-[2-[4-(2-Fluorophenoxymethyl)piperidino]ethyl]-1H-pyrazin-2-one

생성물 1

HCID 222484376-[2-[4-(2-Fluorophenoxymethyl)piperidino]ethyl]-1-methyl-1H-pyrazin-2-one수율 34%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

After dissolving 330 mg of 6-[2-[4-(2-fluorophenoxymethyl)piperidino]ethyl]-1H-pyrazin-2-one in 3 ml of N,N-dimethylformamide, 44 mg of sodium hydride (70% suspension in oil) was added while stirring, and the stirring was continued for 1 hour at room temperature. Next, 0.068 ml of methyl iodide was added and the mixture was stirred overnight at room temperature. Water was added to the reaction solution and extraction was performed with ethyl acetate. The organic layer was washed with water and saturated brine in that order and dried over anhydrous magnesium sulfate, and then the solvent was distilled off under reduced pressure. The residue was purified by NH silica gel column chromatography (solvent: ethyl acetate). Diethyl ether was added and the mixture was filtered to obtain the title compound (116 mg, 34% yield).

후처리

  1. additionwas added
  2. stirringthe mixture was stirred overnight at room temperature
  3. washThe organic layer was washed with water and saturated brine in that order
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled off under reduced pressure
  6. customThe residue was purified by NH silica gel column chromatography (solvent: ethyl acetate)
  7. additionDiethyl ether was added
  8. filtrationthe mixture was filtered

출처 및 근거

ORD 기록
ord-ffe3c69fc3804fb7ac341bcc87cdda41
출처 데이터셋
uspto-grants-2006_02
특허 번호
US06995144B2

반응 노트

불러오는 중…