Dichloroacetyl chloride → 2-(Dichloroacetyl)-1-(1-methylethyl)-4-methyl-1,2,3,4-tetrahydro-isoquinoline

HRID 844950

반응식

HRID 844950 반응식
[CH3:1][CH:2]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)[CH2:3][NH2:4].[C:11](Cl)(=O)[CH:12]([CH3:14])[CH3:13].CC1C2C(=CC=CC=2)CNC1.C1C2C(=CC=CC=2)C=CN=1.[OH-].[Na+].[Cl:40][CH:41]([Cl:45])[C:42](Cl)=[O:43]>O.C(Cl)Cl>[Cl:40][CH:41]([Cl:45])[C:42]([N:4]1[CH2:3][CH:2]([CH3:1])[C:5]2[C:10](=[CH:9][CH:8]=[CH:7][CH:6]=2)[CH:11]1[CH:12]([CH3:14])[CH3:13])=[O:43]

참가 물질

9

반응물 6

HCID 6593Dichloroacetyl chlorideHCID 8405IsoquinolineHCID 113982-PhenylpropylamineHCID 14798Sodium HydroxideHCID 62325Isobutyryl chlorideHCID 137389344-Methyl-1,2,3,4-tetrahydroisoquinoline

생성물 1

HCID 201330432-(Dichloroacetyl)-1-(1-methylethyl)-4-methyl-1,2,3,4-tetrahydro-isoquinoline

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

By procedures described in Example 1 (Method A), β-methyl-phenethylamine and isobutyryl chloride were converted to -4-methyl-1,2,3,4-tetrahydroisoquinoline. A reaction vessel was charged with 3.0 g of this isoquinoline compound, 10 ml 10% sodium hydroxide and 50 ml methylene chloride. With this mixture stirred, 2 ml dichloroacetyl chloride was added dropwise to the mixture. The mixture was stirred for 2 minutes, then water was added. The organic extract was dried with magnesium sulfate and stripped of solvent. The residue was recrystallized from aqueous ethanol to provide 4 g of a white needle-crystalline product having the elemental analysis reported in Table I.

후처리

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

출처 및 근거

ORD 기록
ord-451cd1213c07448ab4fd623420318f8e
출처 데이터셋
uspto-grants-1988_07
특허 번호
US04755218

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