Triethylamine → HCID 23293447, 화합물

HRID 611762노트

반응식

HRID 611762 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 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%.

후처리

  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

출처 및 근거

ORD 기록
ord-111923b33764491498c2cd2aa3710dab
출처 데이터셋
uspto-grants-1999_12
특허 번호
US06001999

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