Phenethylamine → 2-(Dichloroacetyl)-1-phenyl-1,2,3,4-tetrahydroisoquinoline

HRID 844952

反応式

HRID 844952 の反応式
C(N)CC1C=CC=CC=1.C(Cl)(=O)C1C=CC=CC=1.[C:19]1([CH:25]2[C:34]3[C:29](=[CH:30][CH:31]=[CH:32][CH:33]=3)[CH2:28][CH2:27][NH:26]2)[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C1C2C(=CC=CC=2)C=CN=1.[OH-].[Na+].[Cl:47][CH:48]([Cl:52])[C:49](Cl)=[O:50]>O.C(Cl)Cl>[Cl:47][CH:48]([Cl:52])[C:49]([N:26]1[CH2:27][CH2:28][C:29]2[C:34](=[CH:33][CH:32]=[CH:31][CH:30]=2)[CH:25]1[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1)=[O:50]

参加物

9

反応物 6

HCID 1001PhenethylamineHCID 6593Dichloroacetyl chlorideHCID 7412Benzoyl chlorideHCID 8405IsoquinolineHCID 14798Sodium HydroxideHCID 1001371,2,3,4-Tetrahydro-1-phenylisoquinoline

生成物 1

HCID 201330332-(Dichloroacetyl)-1-phenyl-1,2,3,4-tetrahydroisoquinoline

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

By procedures described in Example 1 (Method A), phenethylamine and benzoyl chloride were converted to 1-phenyl-1,2,3,4-tetrahydroisoquinoline. A reaction vessel was charged with 3.5 g of this isoquinoline compound, 10 ml 10% sodium hydroxide and 50 ml methylene chloride. With this mixture stirred, 1.2 ml dichloroacetyl chloride was added dropwise to the mixture. The mixture was stirred for 10 minutes, then water was added. The organic extract was dried with magnesium sulfate and stripped of solvent. The residue was recrystallized from ethanol to provide 4 g of a white cubic-crystal product having the elemental analysis reported in Table I.

後処理

  1. stirringThe mixture was stirred for 10 minutes
  2. extractionThe organic extract
  3. dry with materialwas dried with magnesium sulfate
  4. customThe residue was recrystallized from ethanol

出典と根拠

ORDレコード
ord-12abee4c4ac9483ca98270db7029d4fa
出典データセット
uspto-grants-1988_07
特許番号
US04755218

関連ノート

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