Potassium Iodide → 3-{2-[4-(4-Fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-6-methyl-pyridine-2-carbaldehyde

HRID 11694

반응식

HRID 11694 반응식
[OH:1][C:2]1[C:3]([CH:9]=[O:10])=[N:4][C:5]([CH3:8])=[CH:6][CH:7]=1.Cl[CH2:12][C:13]([N:15]1[CH2:20][C@H:19]([CH3:21])[N:18]([CH2:22][C:23]2[CH:28]=[CH:27][C:26]([F:29])=[CH:25][CH:24]=2)[CH2:17][C@H:16]1[CH3:30])=[O:14].C(=O)([O-])[O-].[K+].[K+].[I-].[K+]>CN(C)C=O.CCOC(C)=O>[F:29][C:26]1[CH:27]=[CH:28][C:23]([CH2:22][N:18]2[C@@H:19]([CH3:21])[CH2:20][N:15]([C:13](=[O:14])[CH2:12][O:1][C:2]3[C:3]([CH:9]=[O:10])=[N:4][C:5]([CH3:8])=[CH:6][CH:7]=3)[C@H:16]([CH3:30])[CH2:17]2)=[CH:24][CH:25]=1

참가 물질

7

반응물 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 113584612-Chloro-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanoneHCID 124219863-Hydroxy-6-methylpyridine-2-carbaldehyde

생성물 1

HCID 865911663-{2-[4-(4-Fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-2-oxo-ethoxy}-6-methyl-pyridine-2-carbaldehyde수율 120.2%

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

반응 조건

온도
60 °C

실험 절차

To a solution of 3-hydroxy-6-methyl-pyridine-2-carbaldehyde (0.27 g, 1.95 mmol) in dimethylformamide (4 mL) was added 2-chloro-1-[4-(4-fluoro-benzyl)-(2R,5S)-2,5-dimethyl-piperazin-1-yl]-ethanone (0.53 g, 1.77 mmol), potassium carbonate (0.49 g, 3.5 mmol) and potassium iodide (0.29 g, 1.8 mmol). The resulting mixture was stirred at 60° C. overnight, then diluted with EtOAc, washed with brine and the organic layer was dried over magnesium sulfate. Filtration followed by concentration in vacuo gave the title compound (0.85 g)

후처리

  1. washwashed with brine
  2. dry with materialthe organic layer was dried over magnesium sulfate
  3. filtrationFiltration
  4. concentrationfollowed by concentration in vacuo

출처 및 근거

ORD 기록
ord-5b57c3e01bd9436dbaed9f98f84c2a35
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07098212B2

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