Triethylamine → HCID 23293447、化合物

HRID 1954663ノート

反応式

HRID 1954663 の反応式
[OH:1][CH2:2][CH2:3][O:4][C:5]1[CH:11]=[CH:10][CH:9]=[CH:8][C:6]=1[NH2:7].Cl[CH2:13][CH2:14][O:15][CH2:16][CH2:17][OH:18].C(N(CC)CC)C>CN(C)C=O>[OH:18][CH2:17][CH2:16][O:15][CH2:14][CH2:13][NH:7][C:6]1[CH:8]=[CH:9][CH:10]=[CH:11][C:5]=1[O:4][CH2:3][CH2:2][OH:1]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 123612-(Chloroethoxy)ethanolHCID 125388802-(2-Amino-phenoxy)-ethanol

生成物 1

HCID 23293447HCID 23293447、化合物収率 53%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
90 °C

実験手順

6 g (39.17 mmol) 2-(2-hydroxyethoxy)aniline A3, 5 ml (5.85 g, 47 mmol) 2-(2-chloroethoxy)ethanol and 8.19 ml (5.95 g, 58.75 mmol) triethylamine were dissolved in 20 ml dimethylformamide and stirred for 4 days at 90° C. After cooling, the solution was filtered, the precipitate washed with dichloromethane and the filtrate concentrated in vacuo. The residue was taken up in chloroform and washed twice with a small quantity of water. The chloroform solution was then dried over sodium sulfate and concentrated. The viscous crude product was purified by column chromatography on silica gel 60 with toluene/acetone 1:2 as the mobile phase. 5 g of brown, viscous oil were obtained; yield 53%.

後処理

  1. temperatureAfter cooling
  2. filtrationthe solution was filtered
  3. washthe precipitate washed with dichloromethane
  4. concentrationthe filtrate concentrated in vacuo
  5. washwashed twice with a small quantity of water
  6. dry with materialThe chloroform solution was then dried over sodium sulfate
  7. concentrationconcentrated
  8. customThe viscous crude product was purified by column chromatography on silica gel 60 with toluene/acetone 1:2 as the mobile phase
  9. custom5 g of brown, viscous oil were obtained

出典と根拠

ORDレコード
ord-3150d7c83b8d4c18ac8a366bfd0dd166
出典データセット
uspto-grants-2000_09
特許番号
US06124135

反応ノート

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