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

HRID 247748
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HRID 247748 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.[ClH:24]>>[ClH:24].[ClH:24].[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

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

생성물 1

HCID 12915163N-methyl-2-amino-alpha-phenylphenethylamine dihydrochloride수율 98%

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온도
100 °C

실험 절차

N-[2-(2-methylamino-2-phenylethyl)phenyl]-2,2-dimethylpropanamide (62 g, 0.2 mol) was dissolved in 6N HCl (124 g) and stirred under a nitrogen atmosphere at 100° C. for 24 hours. The warm reaction mixture (about 35°-40° C.) was extracted with toluene (2×100 ml) to effect recovery of trimethylacetic acid. The aqueous phase was dried by azeotropic distillation with toluene (200 ml) using a Dean-Stark phase separator. The product was collected by filtration, slurried in hot 2-propanol (200 ml), refiltered and dried in vacuo (30 mm) at 45° C. for 12 hours to give N-methyl-2-amino-α-phenylphenethylamine dihydrochloride (58.7 g, 0.196 mol) in 98% yield. The product had a melting point of 251°-253° C.

후처리

  1. customThe warm reaction mixture (about 35°-40° C.)
  2. extractionwas extracted with toluene (2×100 ml)
  3. dry with materialThe aqueous phase was dried by azeotropic distillation with toluene (200 ml)
  4. filtrationThe product was collected by filtration
  5. customdried in vacuo (30 mm) at 45° C. for 12 hours

출처 및 근거

ORD 기록
ord-fb622050f95a4676afd37151dc90bb52
출처 데이터셋
uspto-grants-1987_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04709093

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