Potassium Carbonate → HCID 86666210、化合物

HRID 474667ノート

反応式

HRID 474667 の反応式
[F:1][C:2]1[C:7]([CH3:8])=[CH:6][CH:5]=[C:4]([OH:9])[CH:3]=1.F[C:11]1[CH:18]=[CH:17][C:14]([CH:15]=[O:16])=[CH:13][CH:12]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C.O>[F:1][C:2]1[CH:3]=[C:4]([O:9][C:11]2[CH:18]=[CH:17][C:14]([CH:15]=[O:16])=[CH:13][CH:12]=2)[CH:5]=[CH:6][C:7]=1[CH3:8]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 680234-FluorobenzaldehydeHCID 27746133-Fluoro-4-methylphenol

生成物 1

HCID 86666210HCID 86666210、化合物収率 60.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

反応条件

温度
130 °C

実験手順

To a solution of 3-fluoro-p-cresol (2.5 g, 19.82 mmol) and 4-fluorobenzaldehyde (2.460 g, 19.82 mmol) in DMF (15 mL), was added K2CO3 (4.11 g, 29.7 mmol). The mixture was heated with a microwave condition at 130° C. for 1 h. After cooling, the reaction mixture was diluted in water, extracted with EA. The organic phase was washed with water and brine, dried over Na2SO4, concentrated and purified via flash chromatography to afford the title compound (2.741 g, 11.91 mmol, 60.1% yield) as a yellow oil. LCMS: rt=3.57 min, [M+H+]=231

後処理

  1. temperatureAfter cooling
  2. extractionextracted with EA
  3. washThe organic phase was washed with water and brine
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated
  6. custompurified via flash chromatography

出典と根拠

ORDレコード
ord-5deb8cf538674a40b70337bff58ec0ec
出典データセット
uspto-grants-2014_01
特許番号
US08637536B2

反応ノート

読み込み中…