Triethylamine → HCID 23293447、化合物

HRID 611762ノート

反応式

HRID 611762 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 dichioromethane 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 dichioromethane
  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-111923b33764491498c2cd2aa3710dab
出典データセット
uspto-grants-1999_12
特許番号
US06001999

反応ノート

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