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Ethyl Acrylate → HCID 43365416、化合物

HRID 1991539
ノート
印刷プレビュー

反応式

HRID 1991539 の反応式
[CH2:1]([C:3]1[CH:9]=[CH:8][C:6]([NH2:7])=[CH:5][CH:4]=1)[CH3:2].[C:10]([O:14][CH2:15][CH3:16])(=[O:13])[CH:11]=[CH2:12].[OH-].[Na+]>C(O)(=O)C>[CH2:1]([C:3]1[CH:9]=[CH:8][C:6]([NH:7][CH2:12][CH2:11][C:10]([O:14][CH2:15][CH3:16])=[O:13])=[CH:5][CH:4]=1)[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8821Ethyl Acrylate2 回HCID 115044-EthylanilineHCID 14798Sodium Hydroxide

生成物 1

HCID 43365416HCID 43365416、化合物

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
80 °C

実験手順

To a solution of 4-ethyl aniline (10.0 g) in acetic acid (25 mL) was added ethyl acrylate (10.8 g). The mixture was heated to 80° C. for 2 hours. Additional ethyl acrylate (1.0 mL) was added, and the mixture was again heated to 80° C. for 1 hour. The mixture was allowed to cool to room temperature and stir for two days. Sodium hydroxide (8N) was added until the pH equaled 9. The mixture was partitioned between dichloromethane and water and the combined organics were washed once with 1N sodium hydroxide, once with brine, dried with sodium sulfate, filtered, and concentrated. The mixture was chromatographed using a 20% ethyl acetate in heptane solvent solution. A mixture of the mono and di ester product (19.5 g) were obtained (1:1 mixture). MS (ESI+) for C13H19NO2 m/z 221.99 (M+H)+.

後処理

  1. temperaturethe mixture was again heated to 80° C. for 1 hour
  2. temperatureto cool to room temperature
  3. customThe mixture was partitioned between dichloromethane and water
  4. washthe combined organics were washed once with 1N sodium hydroxide, once with brine
  5. dry with materialdried with sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated
  8. customThe mixture was chromatographed
  9. additionA mixture of the mono and di ester product (19.5 g)
  10. customwere obtained (1:1 mixture)

出典と根拠

ORDレコード
ord-7cae24e54e2e4c698ec1947bdf26079e
出典データセット
uspto-grants-2010_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07645780B2

反応ノート

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