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Water → HCID 18940746、化合物

HRID 356071
ノート
印刷プレビュー

反応式

HRID 356071 の反応式
[C:1]([N:8]([CH2:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=1)[CH2:9][CH2:10][CH2:11][NH:12][C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].[H-].[Na+].[C:30]([N:37]([CH2:40][CH2:41][CH2:42]Br)[CH2:38][CH3:39])([O:32][C:33]([CH3:36])([CH3:35])[CH3:34])=[O:31].O>O1CCOCC1>[CH2:38]([N:37]([C:30]([O:32][C:33]([CH3:35])([CH3:34])[CH3:36])=[O:31])[CH2:40][CH2:41][CH2:42][N:12]([C:13]([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])=[O:14])[CH2:11][CH2:10][CH2:9][N:8]([CH2:20][CH2:21][C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][N:23]=1)[C:1]([O:3][C:4]([CH3:5])([CH3:6])[CH3:7])=[O:2])[CH3:39]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydride2 回HCID 18940742HCID 18940742、化合物HCID 18940749HCID 18940749、化合物2 回

生成物 1

HCID 18940746HCID 18940746、化合物

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

To a solution of 1.85 g (5.1 mmol) of N,N'-di-BOC-N-[2-(2-pyridyl)-ethyl]-1,3-propanediamine in 20 ml of dioxane there are added, with stirring, 0.4 g (10 mmol) of sodium hydride dispersion (approximately 60% in oil; Fluka, Buchs, Switzerland) and, after 20 minutes, a solution of 1.23 ; (6 mmol) of N-BOC-N-ethyl-3-bromo-propylamine in 2 ml of dioxane. The reaction mixture is stirred at 50° C. for 18 hours, a further 0.4 g (10 mmol) of sodium hydride dispersion (approximately 60%) and 1.23 g (6 mmol) of N-BOC-N-ethyl-3-bromo-propylamine are added at 25° C., the mixture is stirred at 50° C. for a further 18 hours and is then coded to room temperature, 50 ml of water are added, and the reaction mixture is extracted with methylene chloride. The methylene chloride extract is dried over sodium sulfate and concentrated by evaporation. and the residue is purified by flash chromatography on silica gel having a particle size of 0.04-0.063 mm using tert-butyl methyl ether. After concentration of the product-containing fractions by evaporation, the title compound is obtained in the form of an oil, Rf value=0.37 (silica gel/tert-butyl methyl ether).

後処理

  1. stirringThe reaction mixture is stirred at 50° C. for 18 hours
  2. stirringthe mixture is stirred at 50° C. for a further 18 hours
  3. customis then coded to room temperature
  4. extractionthe reaction mixture is extracted with methylene chloride
  5. extractionThe methylene chloride extract
  6. dry with materialis dried over sodium sulfate
  7. concentrationconcentrated by evaporation
  8. customand the residue is purified by flash chromatography on silica gel having a particle size of 0.04-0.063 mm
  9. customAfter concentration of the product-containing fractions by evaporation

出典と根拠

ORDレコード
ord-9961d8471781415ab67f76531bbaa7e4
出典データセット
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05834486

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート