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

HRID 247748
ノート
印刷プレビュー

反応式

HRID 247748 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

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

生成物 1

HCID 12915163N-methyl-2-amino-alpha-phenylphenethylamine dihydrochloride収率 98%

反応条件

温度
100 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-fb622050f95a4676afd37151dc90bb52
出典データセット
uspto-grants-1987_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04709093

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート