Potassium Iodide → HCID 117770038、化合物

HRID 1526376

反応式

HRID 1526376 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][NH:6][C:5](=[O:9])[C:4]=1[C:10]#[N:11].C(=O)([O-])[O-].[Cs+].[Cs+].[I-].[K+].Br[CH:21]([CH2:23][CH3:24])[CH3:22]>C(=O)([O-])O.[Na+].COCCOC>[CH:21]([N:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([C:10]#[N:11])[C:5]1=[O:9])([CH2:23][CH3:24])[CH3:22]

参加物

7

反応物 4

HCID 4875Potassium IodideHCID 65542-BromobutaneHCID 10796Cesium carbonateHCID 27867023-Pyridinecarbonitrile, 1,2-dihydro-4-methoxy-2-oxo-

生成物 1

HCID 117770038HCID 117770038、化合物収率 48%

試薬・触媒・溶媒 2

HCID 80711,2-Dimethoxyethane溶媒HCID 516892Sodium Bicarbonate溶媒

反応条件

温度
60 °C

実験手順

To a mixture of 4-methoxy-2-oxo-1,2-dihydropyridine-3-carbonitrile (500 mg), cesium carbonate (2.17 g), potassium iodide (553 mg) N,N-dimethylformamide (10 mL) and 1,2-dimethoxyethane (10 mL) was added 2-bromobutane (776 mg) at room temperature, and the mixture was stirred overnight at 60° C. The reaction mixture was diluted with saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted threetimes with ethyl acetate. The extracts were combined, washed with 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 (ethyl acetate/hexane) to give the title compound (330 mg).

後処理

  1. extractionthe mixture was extracted threetimes with ethyl acetate
  2. washwashed with saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-9d34407f90f241f1a9266b80a887fca7
出典データセット
uspto-grants-2015_07
特許番号
US09085578B2

関連ノート

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