Trifluoroacetic acid → 4-Amino-1-(5-piperid-1-ylcarbonyl-2-pyridyl)piperidine

HRID 23565노트

반응식

HRID 23565 반응식
C(OC([NH:8][CH:9]1[CH2:14][CH2:13][N:12]([C:15]2[CH:20]=[CH:19][C:18]([C:21]([N:23]3[CH2:28][CH2:27][CH2:26][CH2:25][CH2:24]3)=[O:22])=[CH:17][N:16]=2)[CH2:11][CH2:10]1)=O)(C)(C)C.FC(F)(F)C(O)=O>ClCCl>[NH2:8][CH:9]1[CH2:10][CH2:11][N:12]([C:15]2[CH:20]=[CH:19][C:18]([C:21]([N:23]3[CH2:24][CH2:25][CH2:26][CH2:27][CH2:28]3)=[O:22])=[CH:17][N:16]=2)[CH2:13][CH2:14]1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 225744534-Tert-butoxycarbonylamino-1-(5-piperid-1-ylcarbonyl-2-pyridyl)piperidine

생성물 1

HCID 113007004-Amino-1-(5-piperid-1-ylcarbonyl-2-pyridyl)piperidine

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 0.475 g of 4-tert-butoxycarbonylamino-1-(5-piperid-1-ylcarbonyl-2-pyridyl)piperidine (1.24 mmol) and 5 ml of trifluoroacetic acid in 20 ml of dichloromethane is stirred for 1 hour. The reaction medium is concentrated under reduced pressure and then taken up in dichloromethane. The solution is basified (pH=9) using saturated aqueous sodium carbonate solution. The aqueous phase is extracted five times with dichloromethane. The organic phases are dried over magnesium sulfate and concentrated under reduced ressure. The 4-amino-1-(5-piperid-1-ylcarbonyl-2-pyridyl)piperidine is obtained in the form of an oil (0.310 g, 88%). [M+H+]=289.4

후처리

  1. concentrationThe reaction medium is concentrated under reduced pressure
  2. extractionThe aqueous phase is extracted five times with dichloromethane
  3. dry with materialThe organic phases are dried over magnesium sulfate
  4. concentrationconcentrated under reduced ressure

출처 및 근거

ORD 기록
ord-a2f089456b464a99be748955170ba9f6
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06852736B2

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