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

HRID 242639

反応式

HRID 242639 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-ffeff672185d44b5a72d0f69b49de5fa
出典データセット
uspto-grants-2014_02
特許番号
US08653096B2

関連ノート

読み込み中…