tert-Butyl 4-((2-(trifluoromethyl)phenyl)amino)piperidine-1-carboxylate → Piperidin-4-yl-(2-trifluoromethylphenyl)amine

HRID 552129ノート

反応式

HRID 552129 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH:11]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[C:21]([F:24])([F:23])[F:22])[CH2:10][CH2:9]1)=O)(C)(C)C>ClCCl.FC(F)(F)C(O)=O>[NH:8]1[CH2:9][CH2:10][CH:11]([NH:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[C:21]([F:22])([F:23])[F:24])[CH2:12][CH2:13]1

参加物

4

反応物 1

HCID 66591750tert-Butyl 4-((2-(trifluoromethyl)phenyl)amino)piperidine-1-carboxylate

生成物 1

HCID 54902682Piperidin-4-yl-(2-trifluoromethylphenyl)amine収率 99.4%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of 4-(2-trifluoromethylphenylamino)piperidine-1-carboxylic acid tert-butyl ester (0.87 g, 2.52 mmol) in dichloromethane and trifluoroacetic acid (18 mL, 2:1) was stirred at ambient temperature overnight, the solvents were removed by evaporation. The residue was dissolved in ethyl acetate, and the resulting solution was washed with aqueous saturated NaHCO3 and brine, dried over anhydrous Na2SO4 and concentrated to give piperidin-4-yl-(2-trifluoromethylphenyl)amine (0.612 g, 99%) which was used directly for next step reaction without further purification. MS (ES+) m/z 245.0 (M+1).

後処理

  1. customthe solvents were removed by evaporation
  2. dissolutionThe residue was dissolved in ethyl acetate
  3. washthe resulting solution was washed with aqueous saturated NaHCO3 and brine
  4. dry with materialdried over anhydrous Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-44bf684b51304b46bea8dd1d5d60d737
出典データセット
uspto-grants-2011_05
特許番号
US07951805B2

反応ノート

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