tert-Butyl 4-cyano-4-(2,4-dichlorophenyl)piperidine-1-carboxylate → 4-(2,4-Dichlorophenyl)piperidine-4-carbonitrile

HRID 1066998노트

반응식

HRID 1066998 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]([Cl:20])=[CH:16][C:15]=2[Cl:21])[CH2:10][CH2:9]1)=O)(C)(C)C>ClCCl.FC(F)(F)C(O)=O>[Cl:21][C:15]1[CH:16]=[C:17]([Cl: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 49760258tert-Butyl 4-cyano-4-(2,4-dichlorophenyl)piperidine-1-carboxylate

생성물 1

HCID 229935594-(2,4-Dichlorophenyl)piperidine-4-carbonitrile수율 99.6%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

To 4-cyano-4-(2,4-dichlorophenyl)piperidine-1-carboxylic acid tert-butyl ester (0.620 g, 1.74 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 0.442 g (99%) of 4-(2,4-dichlorophenyl)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-70e4be20d47f414e8dd6636afcd8db1d
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06245773B1

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