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

HRID 1158142노트

반응식

HRID 1158142 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 110842664-Fluoro-N-methyl-benzenepropanamine수율 72.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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+).

후처리

  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

출처 및 근거

ORD 기록
ord-7451f565c6c0429b8b8abb2b9fa91d62
출처 데이터셋
uspto-grants-2010_10
특허 번호
US07807720B2

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