Trifluoroacetic acid → N-Benzyl-N-methyl-2-(piperidin-4-yl)ethanamine

HRID 1193336ノート

反応式

HRID 1193336 の反応式
C(O)(C(F)(F)F)=O.[CH2:8]([N:15]([CH3:31])[CH2:16][CH2:17][CH:18]1[CH2:23][CH2:22][N:21](C(OC(C)(C)C)=O)[CH2:20][CH2:19]1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1>ClCCl>[CH2:8]([N:15]([CH3:31])[CH2:16][CH2:17][CH:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1)[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 19261850tert-Butyl 4-(2-(benzyl(methyl)amino)ethyl)piperidine-1-carboxylate

生成物 1

HCID 19085399N-Benzyl-N-methyl-2-(piperidin-4-yl)ethanamine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

TFA (2.78 ml) was added dropwise at 0° C. to a solution of tert-butyl 4-(2-(benzyl(methyl)-amino)ethyl)piperidine-1-carboxylate (600 mg, 1.8 mmol, 1 eq) in dichloromethane (30 ml), and stirring was carried out for 1 h at RT. After monitoring by thin-layer chromatography, the reaction mixture was concentrated to dryness. The residue was dissolved in MeOH (50 ml), Amberlyst A-21 ion-exchanger resin (2 g) was added, and stirring was carried out for 30 min. The reaction mixture was filtered and the filtrate was concentrated to dryness under reduced pressure and used in the next stage without being purified further.

後処理

  1. concentrationthe reaction mixture was concentrated to dryness
  2. dissolutionThe residue was dissolved in MeOH (50 ml)
  3. additionAmberlyst A-21 ion-exchanger resin (2 g) was added
  4. stirringstirring
  5. waitwas carried out for 30 min
  6. filtrationThe reaction mixture was filtered
  7. concentrationthe filtrate was concentrated to dryness under reduced pressure
  8. customwithout being purified further

出典と根拠

ORDレコード
ord-2e3ef4c773794b22ae3c39085d0739a8
出典データセット
uspto-grants-2014_03
特許番号
US08680159B2

反応ノート

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