Dichloroacetyl chloride → 2-(Dichloroacetyl)-1,4,4-trimethyl-1,2,3,4-tetrahydroisoquinoline

HRID 844957

反応式

HRID 844957 の反応式
ClCC(C)(C1C=CC=CC=1)C.[CH3:12][CH:13]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:16]([CH3:24])([CH3:23])[CH2:15][NH:14]1.C1C2C(=CC=CC=2)C=CN=1.[Cl:35][CH:36]([Cl:40])[C:37](Cl)=[O:38].[OH-].[Na+]>C(Cl)Cl.C(#N)C>[Cl:35][CH:36]([Cl:40])[C:37]([N:14]1[CH2:15][C:16]([CH3:23])([CH3:24])[C:17]2[C:22](=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:13]1[CH3:12])=[O:38]

参加物

8

反応物 5

HCID 6593Dichloroacetyl chlorideHCID 8405IsoquinolineHCID 14798Sodium HydroxideHCID 68191Neophyl chlorideHCID 201330451-Methyl-4,4-dimethyl-1,2,3,4-tetrahydroisoquinoline

生成物 1

HCID 201330522-(Dichloroacetyl)-1,4,4-trimethyl-1,2,3,4-tetrahydroisoquinoline

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 6344Dichloromethane溶媒

実験手順

By procedures described in Example 1 (Method B), 1-chloro-2-methyl-2-phenyl-propane and acetonitrile were converted to 1-methyl-4,4-dimethyl-1,2,3,4-tetrahydroisoquinoline. A reaction vessel was charged with 4.0 g of this isoquinoline compound and 50 ml methylene chloride. With this mixture stirred, 2 ml dichloroacetyl chloride was added dropwise to the mixture. The mixture was stirred for 20 minutes and then made alkaline with aqueous sodium hydroxide. The organic extract was dried with magnesium sulfate and stripped of solvent. The residue was recrystallized from ethanol to provide 4.2 g of a white cubic-crystal product having the elemental analysis reported in Table I.

後処理

  1. stirringThe mixture was stirred for 20 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-3dd54f69b57a40fb9d1c7e7449ac6457
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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