Ethyl Bromide → 2-Bromo-5-ethoxypyridine

HRID 76129

反応式

HRID 76129 の反応式
Br[CH2:2][CH3:3].C([O-])([O-])=O.[K+].[K+].[Br:10][C:11]1[CH:16]=[CH:15][C:14]([OH:17])=[CH:13][N:12]=1>C(#N)C>[Br:10][C:11]1[CH:16]=[CH:15][C:14]([O:17][CH2:2][CH3:3])=[CH:13][N:12]=1

参加物

5

反応物 3

HCID 6332Ethyl BromideHCID 11430Potassium CarbonateHCID 27628652-Bromo-5-hydroxypyridine

生成物 1

HCID 234368922-Bromo-5-ethoxypyridine

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

2.51 g (22.99 mmol) 1-bromoethane and 1.99 g (14.37 mmol) K2CO3 are added to a mixture of 1.0 g (5.75 mmol) 2-bromo-5-hydroxypyridine in 100 mL ACN. The mixture is stirred at reflux over night. Then the reaction mixture is poured onto water and extracted with TBME. The organic layer is dried with Na2SO4 and the solvent is removed under vacuo. The residue is purified by column chromatography (silica gel, PE/EtOAC 1/1).

後処理

  1. temperatureat reflux over night
  2. additionThen the reaction mixture is poured onto water
  3. extractionextracted with TBME
  4. dry with materialThe organic layer is dried with Na2SO4
  5. customthe solvent is removed under vacuo
  6. customThe residue is purified by column chromatography (silica gel, PE/EtOAC 1/1)

出典と根拠

ORDレコード
ord-36769e8c1de347da8d1796f0a24d3516
出典データセット
uspto-grants-2014_09
特許番号
US08835472B2

関連ノート

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