Potassium Carbonate → HCID 11241368、化合物

HRID 856587ノート

反応式

HRID 856587 の反応式
C([CH:3]([C:11]1[CH:16]=[C:15]([CH3:17])[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-:19].[K+].[K+]>O>[F:10][C:7]1[CH:8]=[CH:9][C:4]([C:3]([C:11]2[CH:16]=[C:15]([CH3:17])[CH:14]=[CH:13][N:12]=2)=[O:19])=[CH:5][CH:6]=1

参加物

4

反応物 2

HCID 11430Potassium CarbonateHCID 11183726HCID 11183726、化合物

生成物 1

HCID 11241368HCID 11241368、化合物収率 54.3%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

2-(α-cyano-4-fluorobenzyl)-4-methylpyridine (3.1 g) and potassium carbonate (2.9 g) were suspended in 20% hydrated dimethylsulfoxide (150 ml), and the suspension was stirred overnight. The mixture was poured into water, and the mixture was extracted with ethyl acetate. The organic layer was washed with water and saturated brine, dried over anhydrous magnesium sulfate, and then, the solvent was distilled off. The residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane), to give 2-(4-fluorobenzoyl)-4-methylpyridine (1.6 g) as brown crystals.

後処理

  1. extractionthe mixture was extracted with ethyl acetate
  2. washThe organic layer was washed with water and saturated brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off
  5. customThe residue was purified by silica gel column chromatography (elution solvent: ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-11ac5fb20da64060929094e6d82c09f0
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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