Sodium hydride → 3-(2-Octyl)-3-azabicyclo[3.1.0]hexane-2,4-dione

HRID 366539ノート

反応式

HRID 366539 の反応式
[H-].[Na+].[CH:3]12[CH2:8][CH:7]1[C:6](=[O:9])[NH:5][C:4]2=[O:10].Br[CH:12]([CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])[CH3:13]>CN(C)C=O.O>[CH3:13][CH:12]([N:5]1[C:6](=[O:9])[CH:7]2[CH:3]([CH2:8]2)[C:4]1=[O:10])[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 79046Sec-octyl bromide, (+-)-HCID 37200533-Azabicyclo[3.1.0]hexane-2,4-dione

生成物 1

HCID 232899883-(2-Octyl)-3-azabicyclo[3.1.0]hexane-2,4-dione

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

Sodium hydride (0.11 g) was added to a solution of 3-azabicyclo[3.1.0]hexane-2,4-dione (0.3 g) and 2-bromooctane (0.52 g) in dimethylformamide (5 ml) and the resulting mixture was stirred at room temperature under a nitrogen atmosphere for 48 hours. The mixture was diluted with water (15 ml) and then extracted with toluene (20 ml). The organic extract was washed with water (15 ml), dried (MgSO4) and evaporated in vacuo. The residue was purified by Kugelrohr distillation (boiling point 130-140° C. @ 0.1 mmHg) to give the title compound as a colourless oil.

後処理

  1. extractionextracted with toluene (20 ml)
  2. extractionThe organic extract
  3. washwas washed with water (15 ml)
  4. dry with materialdried (MgSO4)
  5. customevaporated in vacuo
  6. distillationThe residue was purified by Kugelrohr distillation (boiling point 130-140° C. @ 0.1 mmHg)

出典と根拠

ORDレコード
ord-161626737cb6480f9d6a0773d0159a65
出典データセット
uspto-grants-2000_10
特許番号
US06130241

反応ノート

読み込み中…