Trifluoroacetic acid → 4-[(2S,5R)-2,5-Dimethylpiperazin-1-yl]-2-fluorobenzonitrile

HRID 1593379노트

반응식

HRID 1593379 반응식
[C:1]([C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C@@H:14]([CH3:15])[CH2:13][N:12](C(OC(C)(C)C)=O)[C@H:11]([CH3:23])[CH2:10]2)=[CH:5][C:4]=1[F:24])#[N:2].FC(F)(F)C(O)=O>ClCCl>[CH3:15][C@H:14]1[CH2:13][NH:12][C@H:11]([CH3:23])[CH2:10][N:9]1[C:6]1[CH:7]=[CH:8][C:3]([C:1]#[N:2])=[C:4]([F:24])[CH:5]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 86601755HCID 86601755, 화합물

생성물 1

HCID 686909784-[(2S,5R)-2,5-Dimethylpiperazin-1-yl]-2-fluorobenzonitrile수율 114.3%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Into 150 ml of dichloromethane was dissolved 15.0 g of tert-butyl (2R,5S)-4-(4-cyano-3-fluorophenyl)-2,5-dimethylpiperazine-1-carboxylate, and then 30 ml of trifluoroacetic acid was added thereto, followed by stirring at room temperature overnight. After the reaction solution was removed by evaporation, 1M hydrochloric acid was added thereto, followed by washing with chloroform. The aqueous phase was made basic with a 5M sodium hydroxide aqueous solution, followed by extraction with chloroform. After the organic layer was dried over anhydrous magnesium sulfate, the solvent was removed by evaporation to obtain 12.0 g of the title compound.

후처리

  1. customAfter the reaction solution was removed by evaporation, 1M hydrochloric acid
  2. additionwas added
  3. washby washing with chloroform
  4. extractionfollowed by extraction with chloroform
  5. dry with materialAfter the organic layer was dried over anhydrous magnesium sulfate
  6. customthe solvent was removed by evaporation

출처 및 근거

ORD 기록
ord-1623394ed6c54c798a53602a02ab42bb
출처 데이터셋
uspto-grants-2007_11
특허 번호
US07297698B2

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