Water → 2-(4-Fluorobenzoyl)-3-propoxypyridine

HRID 856639ノート

反応式

HRID 856639 の反応式
C([CH:3]([C:11]1[C:16]([O:17][CH2:18][CH2:19][CH3:20])=[CH:15][CH:14]=[CH:13][N:12]=1)[C:4]1[CH:9]=[CH:8][C:7]([F:10])=[CH:6][CH:5]=1)#N.C(=O)([O-])[O-:22].[K+].[K+].O>CS(C)=O.O>[F:10][C:7]1[CH:8]=[CH:9][C:4]([C:3]([C:11]2[C:16]([O:17][CH2:18][CH2:19][CH3:20])=[CH:15][CH:14]=[CH:13][N:12]=2)=[O:22])=[CH:5][CH:6]=1

参加物

5

反応物 3

HCID 962WaterHCID 11430Potassium CarbonateHCID 229387622-(alpha-Cyano-4-fluorobenzyl)-3-propoxypyridine

生成物 1

HCID 229388512-(4-Fluorobenzoyl)-3-propoxypyridine収率 85.8%

試薬・触媒・溶媒 1

HCID 23503278(Methanesulfinyl)methane--water (1/1)溶媒

実験手順

Under oxygen atmosphere, a mixed solution of 2-(α-cyano-4-fluorobenzyl)-3-propoxypyridine (5.42 g) and potassium carbonate (3.07 g) in DMSO-water (200-40 ml) was stirred at room temperature for 20 hours. The reaction mixture was added to water and extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate and concentrated under reduced pressure, and the obtained residue was separated and purified by column chromatography (ethyl acetate:hexane 1:3→1:2), to give 2-(4-fluorobenzoyl)-3-propoxypyridine (4.46 g) as pale yellow oil.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with saturated brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customthe obtained residue was separated
  6. custompurified by column chromatography (ethyl acetate:hexane 1:3→1:2)

出典と根拠

ORDレコード
ord-793936c7b05241bdac86b1b253dfbee6
出典データセット
uspto-grants-2007_08
特許番号
US07262185B2

反応ノート

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