Trifluoroacetic acid → Benzyl 2-phenylpiperazine-1-carboxylate

HRID 473817ノート

反応式

HRID 473817 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 16740571Benzyl 2-phenylpiperazine-1-carboxylate収率 94%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

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+).

後処理

  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

出典と根拠

ORDレコード
ord-08fe7b18c6e1455295f2ab95a09a6593
出典データセット
uspto-grants-2014_01
特許番号
US08637499B2

反応ノート

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