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

HRID 23565ノート

反応式

HRID 23565 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-a2f089456b464a99be748955170ba9f6
出典データセット
uspto-grants-2005_02
特許番号
US06852736B2

反応ノート

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