Potassium Sodium Tartrate → N-(2-Chloro-3-trifluoromethylbenzyl)-2-(2-chlorophenyl)propylamine

HRID 902724ノート

反応式

HRID 902724 の反応式
[Cl:1][C:2]1[C:20]([C:21]([F:24])([F:23])[F:22])=[CH:19][CH:18]=[CH:17][C:3]=1[CH2:4][NH:5][C:6](=O)[CH:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[Cl:15])[CH3:8].[H-].C([Al+]CC(C)C)C(C)C.[C@H](O)(C([O-])=O)[C@@H](O)C([O-])=O.[Na+].[K+]>C1(C)C=CC=CC=1.CCCCCC.CCOCC>[Cl:1][C:2]1[C:20]([C:21]([F:24])([F:22])[F:23])=[CH:19][CH:18]=[CH:17][C:3]=1[CH2:4][NH:5][CH2:6][CH:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[Cl:15])[CH3:8]

参加物

7

反応物 3

HCID 9357Potassium Sodium TartrateHCID 21225700DiisobutylaluminumhydrideHCID 69254638N-(2-Chloro-3-trifluoromethylbenzyl)-2-(2-chlorophenyl)propionamide

生成物 1

HCID 69252183N-(2-Chloro-3-trifluoromethylbenzyl)-2-(2-chlorophenyl)propylamine

試薬・触媒・溶媒 3

HCID 1140Toluene溶媒HCID 3283Diethyl Ether溶媒HCID 8058Hexane溶媒

実験手順

A solution of N-(2-chloro-3-trifluoromethylbenzyl)-2-(2-chlorophenyl)propionamide (265 mg, 0.7 mmole) in 40 mL of toluene was treated with diisobutyl aluminum hydride (5 mL of a 1N solution in hexane), and the reaction was stirred for 90 minutes. The reaction was diluted with 20 mL of Et2O, a concentrated aqueous solution of Rochelle salt was added, and the mixture stirred for 60 minutes, at which time the emulsion had broken apart. The organic layer was separated, washed with H2O, aqueous Rochelle salt, dried and the solvent removed, and gave the titled compound, 221 mg (87%). MS (ESI) 362 (MH+).

後処理

  1. stirringthe mixture stirred for 60 minutes, at which time the emulsion
  2. customThe organic layer was separated
  3. washwashed with H2O, aqueous Rochelle salt
  4. customdried
  5. customthe solvent removed

出典と根拠

ORDレコード
ord-c08b500b8b534aef85b5c6e605de45b8
出典データセット
uspto-grants-2008_04
特許番号
US07365085B2

反応ノート

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