HCID 21196091、化合物 → 3-[(5-Bromo-2-fluorophenyl)methoxy]-N-methyl-1-propanamine

HRID 1066844ノート

反応式

HRID 1066844 の反応式
[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]

参加物

3

反応物 1

HCID 21196091HCID 21196091、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-cd9170fd940049fd894b1d51c9c5a63a
出典データセット
uspto-grants-2001_06
特許番号
US06245761B1

反応ノート

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