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

HRID 457163

反応式

HRID 457163 の反応式
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]

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-363384bf4dbc4f68ad8ab2d2e61bd5c8
出典データセット
uspto-grants-2007_03
特許番号
US07186729B2

関連ノート

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