HCID 21196091, 화합물 → 3-[(5-Bromo-2-fluorophenyl)methoxy]-N-methyl-1-propanamine

HRID 1066844노트

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HRID 1066844 반응식
[CH3:1][N:2]([CH2:4][CH2:5][CH2:6][O:7][CH2:8][C:9]1[CH:14]=[C:13]([Br:15])[CH:12]=[CH:11][C:10]=1[F:16])C>ClC(Cl)C>[CH3:1][NH:2][CH2:4][CH2:5][CH2:6][O:7][CH2:8][C:9]1[CH:14]=[C:13]([Br:15])[CH:12]=[CH:11][C:10]=1[F:16]

참가 물질

3

반응물 1

HCID 21196091HCID 21196091, 화합물

생성물 1

HCID 211961783-[(5-Bromo-2-fluorophenyl)methoxy]-N-methyl-1-propanamine

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

In a 15 m flask, under a nitrogen atmosphere, N,N-dimethyl-3-[2-fluoro-5-bromobenzyloxy]propylamine (351 mg, 1.21 mmol) was dissolved in dichloroethane (3.5 ml). To this solution ACE•Cl (0.78 ml, 7.26 mmol) was added and the resulting mixture was heated to reflux and maintained at this temperature for 18 hours. The reaction mixture was cooled to ambient temperature, and the solvents were removed in vacuo. The residue was taken up in methanol and refluxed for 1.5 hours. The methanol solution was then partitioned between 1 M potassium carbonate and methylene chloride. The aqueous fraction was back extracted with methylene chloride. The organic fractions were combined and dried over sodium sulfate. The solvents were removed in vacuo. The title intermediate was further purified by liquid chromatography.

후처리

  1. temperaturethe resulting mixture was heated
  2. temperatureto reflux
  3. temperaturemaintained at this temperature for 18 hours
  4. customthe solvents were removed in vacuo
  5. temperaturerefluxed for 1.5 hours
  6. customThe methanol solution was then partitioned between 1 M potassium carbonate and methylene chloride
  7. extractionThe aqueous fraction was back extracted with methylene chloride
  8. dry with materialdried over sodium sulfate
  9. customThe solvents were removed in vacuo
  10. customThe title intermediate was further purified by liquid chromatography

출처 및 근거

ORD 기록
ord-cd9170fd940049fd894b1d51c9c5a63a
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06245761B1

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