tert-Butyl 4-cyano-4-(2,4-difluorophenyl)piperidine-1-carboxylate → 4-(2,4-Difluorophenyl)-piperidine-4-carbonitrile

HRID 1066995ノート

反応式

HRID 1066995 の反応式
C(OC([N:8]1[CH2:13][CH2:12][C:11]([C:22]#[N:23])([C:14]2[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=2[F:21])[CH2:10][CH2:9]1)=O)(C)(C)C>ClCCl.FC(F)(F)C(O)=O>[F:21][C:15]1[CH:16]=[C:17]([F:20])[CH:18]=[CH:19][C:14]=1[C:11]1([C:22]#[N:23])[CH2:12][CH2:13][NH:8][CH2:9][CH2:10]1

参加物

4

反応物 1

HCID 18353388tert-Butyl 4-cyano-4-(2,4-difluorophenyl)piperidine-1-carboxylate

生成物 1

HCID 105132084-(2,4-Difluorophenyl)-piperidine-4-carbonitrile収率 90%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 6422Trifluoroacetic acid溶媒

実験手順

To 4-Cyano-4-(2,4-difluorophenyl)-piperidine-1-carboxylic acid tert-butyl ester (0.720 g, 2.42 mmol) in 5 ml of dichloromethane, 2 ml of trifluoroacetic acid was added and the solution stirred at room temperature for 1 hour. The solution was concentrated, neutralized with 10% KOH solution and extracted into 25 ml of dichloromethane. The organic layer was dried over sodium sulfate, filtered and concentrated to give 0.484 g (90%) of 4-(2,4-difluorophenyl)-piperidine-4-carbonitrile which was used as such for the subsequent step.

後処理

  1. concentrationThe solution was concentrated
  2. extractionextracted into 25 ml of dichloromethane
  3. dry with materialThe organic layer was dried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-9556294d98604d2dbe3c922a4a0f0935
出典データセット
uspto-grants-2001_06
特許番号
US06245773B1

反応ノート

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