Ethanolamine → HCID 49854108、化合物

HRID 2410611ノート

反応式

HRID 2410611 の反応式
[CH2:1]([CH2:3][NH2:4])[OH:2].C([O:7][C:8](=O)[C:9]([C:11]1[CH:19]=[CH:18][C:14]2[O:15][CH2:16][O:17][C:13]=2[CH:12]=1)=[O:10])C>C(O)C>[O:15]1[C:14]2[CH:18]=[CH:19][C:11]([C:9](=[O:10])[C:8]([NH:4][CH2:3][CH2:1][OH:2])=[O:7])=[CH:12][C:13]=2[O:17][CH2:16]1

参加物

4

反応物 2

HCID 700EthanolamineHCID 2758872Ethyl (2H-1,3-benzodioxol-5-yl)(oxo)acetate

生成物 1

HCID 49854108HCID 49854108、化合物収率 34.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethanolamine (3.5 g, 49 mmol) was added to a stirred solution of benzo[1,3]dioxol-5-yl-oxo-acetic acid ethyl ester (2.5 g, 11 mmol)) in ethanol (40 ml)) at room temperature. The resulting reaction mixture was heated to reflux for 2 hours. Then ethanol was distilled off and stirring was continued at 120° C. for 1 hour. The reaction mixture was cooled to room temperature and then 50 ml of THF and 100 ml of aqueous HCl solution were added and stirred for 30 minutes. The mixture was extracted twice with DCM (50 ml). The organic layer was washed twice with water (50 ml) and evaporated to provide a dark sticky product. The product was further crystallized in pentane/ethyl acetate. Red crystals of the title compound (0.9 g, 34.5% yield) were obtained.

後処理

  1. customThe resulting reaction mixture
  2. temperaturewas heated
  3. temperatureto reflux for 2 hours
  4. distillationThen ethanol was distilled off
  5. addition50 ml of THF and 100 ml of aqueous HCl solution were added
  6. stirringstirred for 30 minutes
  7. extractionThe mixture was extracted twice with DCM (50 ml)
  8. washThe organic layer was washed twice with water (50 ml)
  9. customevaporated
  10. customto provide a dark sticky product
  11. customThe product was further crystallized in pentane/ethyl acetate

出典と根拠

ORDレコード
ord-50f64143aeba44c78ac2d0fccdb0ace4
出典データセット
uspto-grants-2014_08
特許番号
US08816102B2

反応ノート

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