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

HRID 1193336노트

반응식

HRID 1193336 반응식
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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2e3ef4c773794b22ae3c39085d0739a8
출처 데이터셋
uspto-grants-2014_03
특허 번호
US08680159B2

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