Trifluoroacetic acid → 5-Chloro-2-(piperazin-1-yl)benzonitrile

HRID 557031

반응식

HRID 557031 반응식
C(OC([N:8]1[CH2:13][CH2:12][N:11]([C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][C:15]=2[C:21]#[N:22])[CH2:10][CH2:9]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[Cl:20][C:17]1[CH:18]=[CH:19][C:14]([N:11]2[CH2:10][CH2:9][NH:8][CH2:13][CH2:12]2)=[C:15]([CH:16]=1)[C:21]#[N:22]

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 667578634-(4-Chloro-2-cyano-phenyl)-piperazine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 193671275-Chloro-2-(piperazin-1-yl)benzonitrile

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 4-(4-chloro-2-cyano-phenyl)-piperazine-1-carboxylic acid tert-butyl ester (0.32 g, 1 mmol) in dichloromethane cooled at 0° C. was treated with trifluoroacetic acid (20%) and warmed to room temperature and stirred for 2 h. The reaction mixture was concentrated in vacuo, diluted with ethyl acetate and free based with 10% aqueous sodium bicarbonate. The organic layers were separated and dried over sodium sulfate and concentrated in vacuo. The product used without further purification.

후처리

  1. concentrationThe reaction mixture was concentrated in vacuo
  2. additiondiluted with ethyl acetate
  3. customThe organic layers were separated
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated in vacuo
  6. customThe product used without further purification

출처 및 근거

ORD 기록
ord-15d475cc9307404a9bf3109fd7d26853
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08058287B2

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