Trifluoroacetic acid → Benzyl 2-phenylpiperazine-1-carboxylate

HRID 473817노트

반응식

HRID 473817 반응식
[C:1]1([CH:7]2[CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][CH2:9][N:8]2[C:20]([O:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)=[O:21])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.FC(F)(F)C(O)=O>ClCCl>[C:1]1([CH:7]2[CH2:12][NH:11][CH2:10][CH2:9][N:8]2[C:20]([O:22][CH2:23][C:24]2[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=2)=[O:21])[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 675145701-Benzyl 4-tert-butyl 2-phenylpiperazine-1,4-dicarboxylate

생성물 1

HCID 16740571Benzyl 2-phenylpiperazine-1-carboxylate수율 94%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
25 °C

실험 절차

To 1-benzyl 4-tert-butyl 2-phenylpiperazine-1,4-dicarboxylate (0.84 g, 2.12 mmol) in dichloromethane (5.0 mL) added drop wise trifluoroacetic acid (5.0 mL) and maintained at 25° C. for 90 minutes. The reaction mixture was concentrated, and the residue dissolved in ethyl acetate (60 mL). The solution was washed with saturated aqueous sodium carbonate (30 mL) and brine (20 mL), and then dried over anhydrous sodium sulfate, filtered and concentrated to yield benzyl 2-phenylpiperazine-1-carboxylate (0.59 g, 94% yield). MS (EI) for C18H20N2O2: 297 (MH+).

후처리

  1. concentrationThe reaction mixture was concentrated
  2. dissolutionthe residue dissolved in ethyl acetate (60 mL)
  3. washThe solution was washed with saturated aqueous sodium carbonate (30 mL) and brine (20 mL)
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-08fe7b18c6e1455295f2ab95a09a6593
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637499B2

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