Triethylamine → HCID 23293447, 화합물

HRID 1954663노트

반응식

HRID 1954663 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

HCID 23293447HCID 23293447, 화합물수율 53%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
90 °C

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-3150d7c83b8d4c18ac8a366bfd0dd166
출처 데이터셋
uspto-grants-2000_09
특허 번호
US06124135

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