Butyl bromide → HCID 59234227、化合物

HRID 1400203ノート

反応式

HRID 1400203 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].Br[CH2:13][CH2:14][CH2:15][CH3:16].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[CH2:13]([N:6]1[CH:7]=[CH:8][C:3]([O:2][CH3:1])=[C:4]([C:10]#[N:11])[C:5]1=[O:9])[CH2:14][CH2:15][CH3:16]

参加物

5

反応物 3

HCID 8002Butyl bromideHCID 11430Potassium CarbonateHCID 27867023-Pyridinecarbonitrile, 1,2-dihydro-4-methoxy-2-oxo-

生成物 1

HCID 59234227HCID 59234227、化合物収率 99.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

反応条件

温度
110 °C

実験手順

To a solution of 4-methoxy-2-oxo-1,2-dihydro-pyridine-3-carbonitrile (20 g, 133 mmol) in acetonitrile (800 ml) were added 1-bromobutane (15.8 ml, 146 mmol) and potassium carbonate (36.7 g, 266 mmol) and the mixture was heated at 110° C. for 24 hours. The mixture was cooled to room temperature and the solid was filtered off The filtrate was evaporated till dryness and the resulting crude residue was then triturated with diethylether to yield pure intermediate 4 (27.39 g, >99%) as a white solid.

後処理

  1. temperatureThe mixture was cooled to room temperature
  2. filtrationthe solid was filtered off The filtrate
  3. customwas evaporated till dryness
  4. customthe resulting crude residue was then triturated with diethylether

出典と根拠

ORDレコード
ord-2d3089667ecd46d0abd5110fe40970dd
出典データセット
uspto-grants-2014_12
特許番号
US08906939B2

反応ノート

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