Trifluoroacetic acid → HCID 61632462、化合物

HRID 1477586ノート

反応式

HRID 1477586 の反応式
[F:1][C:2]([F:22])([F:21])[C:3]1[CH:7]=[CH:6][N:5]([CH:8]2[CH2:13][CH2:12][N:11](C(OC(C)(C)C)=O)[CH2:10][CH2:9]2)[N:4]=1.FC(F)(F)C(O)=O>ClCCl>[F:22][C:2]([F:1])([F:21])[C:3]1[CH:7]=[CH:6][N:5]([CH:8]2[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]2)[N:4]=1

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 712265361-Piperidinecarboxylic acid, 4-[3-(trifluoromethyl)-1H-pyrazol-1-yl]-, 1,1-dimethylethyl ester

生成物 1

HCID 61632462HCID 61632462、化合物収率 127.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a dichloromethane solution (1.5 mL) of tert-butyl 4-[3-(trifluoromethyl)-1H-pyrazol-1-yl]piperidine-1-carboxylate (150 mg, 0.50 mmol) synthesized in Reference Synthesis Example 33, trifluoroacetic acid (0.7 mL) was added at room temperature, and the resultant solution was stirred for 3 hours. After completion of the reaction, the reaction solution was concentrated under reduced pressure and water was added to the concentrated reaction solution, followed by extraction from the resultant mixture with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to obtain the title compound (140 mg, quantitative).

後処理

  1. additionwas added at room temperature
  2. customAfter completion of the reaction
  3. concentrationthe reaction solution was concentrated under reduced pressure and water
  4. additionwas added to the concentrated reaction solution
  5. extractionfollowed by extraction from the resultant mixture with ethyl acetate
  6. washThe organic layer was washed with brine
  7. dry with materialdried over anhydrous sodium sulfate
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-94a0f81f217243a6bf86df6525b05066
出典データセット
uspto-grants-2016_08
特許番号
US09403798B2

反応ノート

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