Trifluoroacetic acid → Dimethyl-(4-piperazin-1-YL-phenyl)-amine

HRID 1647394노트

반응식

HRID 1647394 반응식
FC(F)(F)C(O)=O.C(OC([N:15]1[CH2:20][CH2:19][N:18]([C:21]2[CH:26]=[CH:25][C:24]([N:27]([CH3:29])[CH3:28])=[CH:23][CH:22]=2)[CH2:17][CH2:16]1)=O)(C)(C)C>ClCCl>[CH3:28][N:27]([CH3:29])[C:24]1[CH:23]=[CH:22][C:21]([N:18]2[CH2:19][CH2:20][NH:15][CH2:16][CH2:17]2)=[CH:26][CH:25]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 226678081-(Tert-butoxycarbonyl)-4-(4-dimethylaminophenyl)piperazine

생성물 1

HCID 4738754Dimethyl-(4-piperazin-1-YL-phenyl)-amine수율 84.4%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Trifluoroacetic acid (10 ml) was added to a solution of 1-(tert-butoxycarbonyl)-4-(4-dimethylaminophenyl)piperazine (2.01 g 6.58 mmol ) in dichloromethane (20 ml) and the mixture stirred for 30 min at room temperature. The mixture was concentrated in vacuo and saturated aqueous potassium carbonate (100 ml) was cautiously added to the residue. The mixture was extracted with dichloromethane (3×100 ml), the extracts were washed with brine (50 ml), combined and dried (MgSO4). Concentration of the extracts gave 1-(4-dimethylaminophenyl)piperazine (1.14 g, 84%) as a cream solid; δH (DMSO-d6) 2.77 (6H, s, N(CH3)2), 2.79 (4H, m, 2×piperazinyl CH2), 2.86 (4H, m, 2×piperazinyl CH2), 6.68 (2H, m, ArH), and 6.82 (2H, m, ArH).

후처리

  1. concentrationThe mixture was concentrated in vacuo and saturated aqueous potassium carbonate (100 ml)
  2. additionwas cautiously added to the residue
  3. extractionThe mixture was extracted with dichloromethane (3×100 ml)
  4. washthe extracts were washed with brine (50 ml)
  5. dry with materialdried (MgSO4)

출처 및 근거

ORD 기록
ord-fcf7bd6b8fd14203bb9d817f1af4f956
출처 데이터셋
uspto-grants-1995_07
특허 번호
US05432177

반응 노트

불러오는 중…