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

HRID 366539노트

반응식

HRID 366539 반응식
[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]

참가 물질

6

반응물 3

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-161626737cb6480f9d6a0773d0159a65
출처 데이터셋
uspto-grants-2000_10
특허 번호
US06130241

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