Trifluoroacetic acid → 4-Fluoro-N-methyl-benzenepropanamine

HRID 1158142ノート

反応式

HRID 1158142 の反応式
C(O[C:6](=O)[N:7]([CH2:9][CH2:10][CH2:11][C:12]1[CH:17]=[CH:16][C:15]([F:18])=[CH:14][CH:13]=1)C)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[F:18][C:15]1[CH:14]=[CH:13][C:12]([CH2:11][CH2:10][CH2:9][NH:7][CH3:6])=[CH:17][CH:16]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 59512610[3-(4-Fluoro-phenyl)-propyl]-methyl-carbamic acid tert-butyl ester

生成物 1

HCID 110842664-Fluoro-N-methyl-benzenepropanamine収率 72.5%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of [3-(4-fluoro-phenyl)-propyl]-methyl-carbamic acid tert-butyl ester (0.417 g, 1.560 mmol) in 3 mL of dichloromethane, was added trifluoroacetic acid (3 mL). After stirring at room temperature for 3 h, the reaction mixture was concentrated under reduced pressure. The residue was re-dissolved in 20 mL of ethyl acetate and the resulting solution was washed with NaOH solution (1N) and brine, and dried over anhydrous Na2SO4. Removal of the solvent under reduced pressure provided the title compound as a colorless oil (0.189 g, 72% yield), which was used directly in the next step (Step d of Specific Scheme 7) without further purification. GC-MS: tR=5.6 min; m/z 167 (M+).

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. dissolutionThe residue was re-dissolved in 20 mL of ethyl acetate
  3. washthe resulting solution was washed with NaOH solution (1N) and brine
  4. dry with materialdried over anhydrous Na2SO4
  5. customRemoval of the solvent under reduced pressure

出典と根拠

ORDレコード
ord-7451f565c6c0429b8b8abb2b9fa91d62
出典データセット
uspto-grants-2010_10
特許番号
US07807720B2

反応ノート

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