Potassium Carbonate → 3-n-Decyl-3-azabicyclo[3.1.0]hexane-2,4-dione

HRID 366531

反応式

HRID 366531 の反応式
I[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].[CH:12]12[CH2:17][CH:16]1[C:15](=[O:18])[NH:14][C:13]2=[O:19].C(=O)([O-])[O-].[K+].[K+]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.ClCCl>[CH2:2]([N:14]1[C:15](=[O:18])[CH:16]2[CH:12]([CH2:17]2)[C:13]1=[O:19])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 163141-IododecaneHCID 37200533-Azabicyclo[3.1.0]hexane-2,4-dione

生成物 1

HCID 232899843-n-Decyl-3-azabicyclo[3.1.0]hexane-2,4-dione

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 6344Dichloromethane溶媒

実験手順

1-Iododecane (1.21 g) was added to a stirred mixture of 3-azabicyclo[3.1.0]hexane-2,4 dione (0.5 g), potassium carbonate (0.62 g) and tetrabutylammonium bromide (1.45 g) in dichloromethane (50 ml) at room temperature and the resulting mixture was stirred for 24 hours. The mixture was filtered and the filtrate was then washed with water (2×100 ml), dried (MgSO4) and evaporated in vacuo to give a brown oil. The oil was purified by column chromatography on silica gel (100 g) using hexane as eluant. Combination and evaporation of the appropriate fractions gave the title compound as a colourless oil.

後処理

  1. filtrationThe mixture was filtered
  2. washthe filtrate was then washed with water (2×100 ml)
  3. dry with materialdried (MgSO4)
  4. customevaporated in vacuo
  5. customto give a brown oil
  6. customThe oil was purified by column chromatography on silica gel (100 g)
  7. customCombination and evaporation of the appropriate fractions

出典と根拠

ORDレコード
ord-b6791d355ab8451faf9e7b93158ea257
出典データセット
uspto-grants-2000_10
特許番号
US06130241

関連ノート

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