Potassium Carbonate → HCID 67383896、化合物

HRID 408110

反応式

HRID 408110 の反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[NH:9][C:10](=[O:12])[CH3:11])[CH3:2].C([O-])([O-])=O.[K+].[K+].Br[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[CH2:26][CH3:27]>[Cu]Br>[CH2:1]([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[N:9]([C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=1[CH2:26][CH3:27])[C:10](=[O:12])[CH3:11])[CH3:2]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 160891-Bromo-2-ethylbenzeneHCID 36332O-Ethylacetanilide

生成物 1

HCID 67383896HCID 67383896、化合物収率 67%

試薬・触媒・溶媒 1

HCID 24593copper(I) bromide触媒

反応条件

温度
200 °C

実験手順

The mixture of the N-(2-ethylphenyl)acetamide (7.35 g, 45.03 mmol), anhydrous K2CO3 (6.22 g, 45.03 mmol), copper(I) bromide (452.2 mg, 3.15 mmol) in 1-bromo-2-ethylbenzene was stirred and heated to 200° C. under argon for 48 h. After cooling the reaction mixture was poured into ice-H2O and extracted with ethyl acetate (2×500 mL), the combined organics were washed with brine, dried over anhydrous (K2CO3), filtered and concentrated to dryness. The crude product was purified using an ISCO machine using a ethyl acetate-hexane gradient to afford the product, N,N-bis(2-ethylphenyl)acetamide (8.1 g, 67%).

後処理

  1. temperatureAfter cooling the reaction mixture
  2. extractionextracted with ethyl acetate (2×500 mL)
  3. washthe combined organics were washed with brine
  4. dry with materialdried over anhydrous (K2CO3)
  5. filtrationfiltered
  6. concentrationconcentrated to dryness
  7. customThe crude product was purified

出典と根拠

ORDレコード
ord-c6783476024348b39cf8721dedd375c9
出典データセット
uspto-grants-2014_06
特許番号
US08759336B2

関連ノート

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