Diethylamine → 3-(Boc-amino)piperidine

HRID 501411ノート

反応式

HRID 501411 の反応式
C(NCC)C.[C:6]([O:10][C:11]([NH:13][CH:14]1[CH2:19][CH2:18][CH2:17][N:16](C(OCC2C3C=CC=CC=3C3C2=CC=CC=3)=O)[CH2:15]1)=[O:12])([CH3:9])([CH3:8])[CH3:7]>C(O)C>[NH:16]1[CH2:17][CH2:18][CH2:19][CH:14]([NH:13][C:11](=[O:12])[O:10][C:6]([CH3:8])([CH3:7])[CH3:9])[CH2:15]1

参加物

4

反応物 2

HCID 8021DiethylamineHCID 23070937HCID 23070937、化合物

生成物 1

HCID 42330413-(Boc-amino)piperidine収率 88.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

25 ml of diethylamine was added to 250 ml of an ethanol solution of 1.88 g of 9H-fluoren-9-ylmethyl 3-t-butoxycarbonylaminopiperidine-1-carboxylate, and the mixture was stirred at room temperature for 18 hours. After the solution had been concentrated under reduced pressure, the residue was dissolved in a mixture consisting of 150 ml of toluene and 100 ml of 10% aqueous citric acid solution. The aqueous layer was made alkaline with a 5N aqueous sodium hydroxide solution, and then extracted twice with 100 ml of dichloromethane. The organic layers were combined together, dried over anhydrous magnesium sulfate, and concentrated under reduced pressure to give 0.79 g of the title compound.

後処理

  1. concentrationAfter the solution had been concentrated under reduced pressure
  2. dissolutionthe residue was dissolved in a mixture
  3. extractionextracted twice with 100 ml of dichloromethane
  4. dry with materialdried over anhydrous magnesium sulfate
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-d8aeda4238644949a7c71f8691229e49
出典データセット
uspto-grants-2010_08
特許番号
US07772226B2

反応ノート

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