N-Methylephedrine → Metamfepramone

HRID 1721534

반응식

HRID 1721534 반응식
[CH3:1][CH:2]([N:11]([CH3:13])[CH3:12])[CH:3]([OH:10])[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.I(C1C=CC=CC=1C(O)=O)(=O)=O.FC(F)(F)C(O)=O>CS(C)=O.C([O-])(O)=O.[Na+]>[CH3:12][N:11]([CH3:13])[CH:2]([CH3:1])[C:3]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)=[O:10]

참가 물질

6

반응물 3

HCID 4374N-MethylephedrineHCID 6422Trifluoroacetic acidHCID 1087942-Iodoxybenzoic acid

생성물 1

HCID 71872Metamfepramone수율 90.7%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 516892Sodium Bicarbonate용매

실험 절차

N-Methylephedrine (200 mg; 1.12 mmol) was added to a solution of o-iodoxybenzoic acid I (1.56 g, 5.59 mmol) and trifluoroacetic acid (0.13 ml) in DMSO (12 ml). After 8 hours the solution was diluted with NaHCO3 (2.5%, 30 ml) and extracted with ethyl acetate (3×10 ml). The combined organic layers were washed with water (2×5 ml), dried over sodium sulfate and evaporated to dryness under vacuum to give 180 mg (90%) of 2-dimethylamino-1-phenyl-propan-1-one identical to the sample obtained in Example 31.

후처리

  1. extractionextracted with ethyl acetate (3×10 ml)
  2. washThe combined organic layers were washed with water (2×5 ml)
  3. dry with materialdried over sodium sulfate
  4. customevaporated to dryness under vacuum

출처 및 근거

ORD 기록
ord-e1d12438905c4b90822c0531f7a304da
출처 데이터셋
uspto-grants-1996_04
특허 번호
US05510538

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