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

HRID 1066995노트

반응식

HRID 1066995 반응식
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

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9556294d98604d2dbe3c922a4a0f0935
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06245773B1

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