Trifluoroacetic acid → 1-(4-Diisopropylaminomethylbenzoyl)piperazine

HRID 278549노트

반응식

HRID 278549 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14](=[O:29])[C:15]2[CH:20]=[CH:19][C:18]([CH2:21][N:22]([CH:26]([CH3:28])[CH3:27])[CH:23]([CH3:25])[CH3:24])=[CH:17][CH:16]=2)[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>C(OCC)(=O)C>[CH:23]([N:22]([CH2:21][C:18]1[CH:19]=[CH:20][C:15]([C:14]([N:11]2[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]2)=[O:29])=[CH:16][CH:17]=1)[CH:26]([CH3:28])[CH3:27])([CH3:24])[CH3:25]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 226280611-(Tert-butoxycarbonyl)-4-(4-diisopropylaminomethylbenzoyl)piperazine

생성물 1

HCID 226279521-(4-Diisopropylaminomethylbenzoyl)piperazine수율 90.2%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 1-(tert-butoxycarbonyl)-4-(4-diisopropylaminomethylbenzoyl)piperazine (4.6 g) in ethyl acetate (10 ml) was added trifluoroacetic acid (20 ml), and the solution was stirred at room temperature for 1 hour and concentrated. The residue was dissolved in water. The solution was made alkaline with sodium hydroxide solution, extracted with dichloromethane. The extract was dried and concentrated to give amorphous powders which were filtered, washed with hexane and dried to afford the title compound (3.12 g).

후처리

  1. concentrationconcentrated
  2. dissolutionThe residue was dissolved in water
  3. extractionextracted with dichloromethane
  4. customThe extract was dried
  5. concentrationconcentrated
  6. customto give amorphous powders which
  7. filtrationwere filtered
  8. washwashed with hexane
  9. customdried

출처 및 근거

ORD 기록
ord-084ef76c38a54aa4b696a7f2a3824efa
출처 데이터셋
uspto-grants-2002_03
특허 번호
US06359134B1

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