Diethanolamine → HCID 11770129、化合物

HRID 1928537ノート

反応式

HRID 1928537 の反応式
[OH:1][CH2:2][CH2:3][NH:4][CH2:5][CH2:6][OH:7].Br[CH2:9][CH2:10][O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[OH:1][CH2:2][CH2:3][N:4]([CH2:9][CH2:10][O:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1)[CH2:5][CH2:6][OH:7]

参加物

5

反応物 3

HCID 8113DiethanolamineHCID 11430Potassium CarbonateHCID 68526Benzene, (2-bromoethoxy)-

生成物 1

HCID 11770129HCID 11770129、化合物収率 78%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The reaction mixture of 2-(2-hydroxy-ethylamino)ethanol (32 g, 310 mmol), 1-(2-bromoethoxy)benzene (51 g, 256 mmol), and potassium carbonate (70 g, 512 mmol) in ethanol (200 mL) was refluxed overnight, concentrated, and partitioned between water and ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by column chromatography to afford the title compound (45 g, 78%).

後処理

  1. temperaturewas refluxed overnight
  2. concentrationconcentrated
  3. custompartitioned between water and ethyl acetate
  4. washThe organic layer was washed with brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated
  7. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-ce6f958296a34e70b8b597c0f29faa50
出典データセット
uspto-grants-2012_05
特許番号
US08183374B2

反応ノート

読み込み中…