Potassium Carbonate → 2-(2-bromophenyl)-N-(2-ethoxyethyl)ethanamine

HRID 387641노트

반응식

HRID 387641 반응식
CS(O[CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[Br:14])(=O)=O.[CH2:15]([O:17][CH2:18][CH2:19][NH2:20])[CH3:16].C(=O)([O-])[O-].[K+].[K+]>O1CCCC1>[Br:14][C:9]1[CH:10]=[CH:11][CH:12]=[CH:13][C:8]=1[CH2:7][CH2:6][NH:20][CH2:19][CH2:18][O:17][CH2:15][CH3:16]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 66970EthoxyethylamineHCID 15364878HCID 15364878, 화합물

생성물 1

HCID 684705122-(2-bromophenyl)-N-(2-ethoxyethyl)ethanamine

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

3.5 g of 2-(2-bromophenyl)ethyl methanesulfonate, 5.59 g of 2-ethoxyethanamine, 8.67 g of potassium carbonate and 70 cm3 of tetrahydrofuran are stirred under the reflux of the solvent under an inert atmosphere for 48 h. The heating is stopped, then the reaction mixture is filtered. The insoluble material is washed twice with ethyl acetate. The filtrate is concentrated using a rotary evaporator under reduced pressure (5 kPa). The product obtained is purified by flash chromatography over silica (column: 330 g; particle size: 20-40 μm, spherical; eluent: 100% ethyl acetate to 90% ethyl acetate/10% methanol gradient). After concentrating the fractions under reduced pressure, 2.45 g of 2-(2-bromophenyl)-N-(2-ethoxyethyl)ethanamine are obtained in the form of a yellow oil.

후처리

  1. temperaturereflux of the solvent under an inert atmosphere for 48 h
  2. filtrationthe reaction mixture is filtered
  3. washThe insoluble material is washed twice with ethyl acetate
  4. concentrationThe filtrate is concentrated
  5. customa rotary evaporator under reduced pressure (5 kPa)
  6. customThe product obtained
  7. customis purified by flash chromatography over silica (column: 330 g; particle size: 20-40 μm, spherical; eluent: 100% ethyl acetate to 90% ethyl acetate/10% methanol gradient)
  8. concentrationAfter concentrating the fractions under reduced pressure, 2.45 g of 2-(2-bromophenyl)-N-(2-ethoxyethyl)ethanamine
  9. customare obtained in the form of a yellow oil

출처 및 근거

ORD 기록
ord-ec8a03b675bb4e06be24ae3e8cea9adb
출처 데이터셋
uspto-grants-2013_02
특허 번호
US08372864B2

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