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Hydrochloric Acid → N-methyl-2-amino-alpha-phenylphenethylamine dihydrochloride

HRID 1462850
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HRID 1462850 반응식
[CH3:1][NH:2][CH:3]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH:11]C(=O)C(C)(C)C.C1(C)C=CC=CC=1.[ClH:31]>>[ClH:31].[ClH:31].[CH3:1][NH:2][CH:3]([C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1)[CH2:4][C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=1[NH2:11]
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참가 물질

4

반응물 3

HCID 313Hydrochloric AcidHCID 1140TolueneHCID 10968937N-[2-(2-methylamino-2-phenylethyl)phenyl]-2,2-dimethylpropanamide

생성물 1

HCID 12915163N-methyl-2-amino-alpha-phenylphenethylamine dihydrochloride수율 93%

반응 조건

온도
100 °C

실험 절차

N-[2-(2-methylamino-2-phenylethyl)phenyl]-2,2-dimethyl-propanamide (155 g, 0.5 mol) was dissolved in 6N HCl (310 g) and stirred under a nitrogen atmosphere at 100° C. for 28 hours. The reaction mixture was cooled to 23° C. and toluene (200 ml) was added. Stirring was continued until the product had crystallized from the aqueous phase. The product was collected by filtration, washed with toluene (2×50 ml) and dried in vacuo (30 mm) at 60° C. for 60 hours to give N-methyl-2-amino-α-phenylphenethylamine dihydrochloride (139 g, 93% yield). The melting point of the product was 252°-254° C. The organic phase of the filtrate was concentrated in vacuo to give a 58% recovery of trimethylacetic acid. The aqueous phase of the filtrate afforded a second crop of N-methyl-2-amino-α-phenylphenethylamine dihydrochloride (9.3 g, 6%). The total yield of product was 99%.

후처리

  1. temperatureThe reaction mixture was cooled to 23° C.
  2. stirringStirring
  3. customhad crystallized from the aqueous phase
  4. filtrationThe product was collected by filtration
  5. washwashed with toluene (2×50 ml)
  6. customdried in vacuo (30 mm) at 60° C. for 60 hours

출처 및 근거

ORD 기록
ord-c3949302cfe345e69d634a34ce48d049
출처 데이터셋
uspto-grants-1984_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04461728

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