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

反応式

HRID 11694 の反応式
[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

参加物

7

反応物 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

生成物 1

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

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
60 °C

実験手順

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)

後処理

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

出典と根拠

ORDレコード
ord-5b57c3e01bd9436dbaed9f98f84c2a35
出典データセット
uspto-grants-2006_08
特許番号
US07098212B2

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