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Chemical Structure| 280-97-7 Chemical Structure| 280-97-7

Structure of 280-97-7

Chemical Structure| 280-97-7

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Product Details of [ 280-97-7 ]

CAS No. :280-97-7
Formula : C8H15N
M.W : 125.21
SMILES Code : C1(N2)CCCC2CCC1
MDL No. :MFCD07780803

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Application In Synthesis of [ 280-97-7 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 280-97-7 ]

[ 280-97-7 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 280-97-7 ]
  • [ 31785-68-9 ]
YieldReaction ConditionsOperation in experiment
80% With sodium tungstate (VI) dihydrate; urea hydrogen peroxide adduct; In water; at 0 - 20℃; for 2h; Add water (600 mL) to the reaction solution from the previous step, cool to 0-10C in an ice water bath, add sodium tungstate dihydrate (30.6 g), and add carbamide peroxide (170.5 g) in batches. After adding, it will naturally rise to room temperature. After reaction for 2h, samples were taken and tested, and the reaction was complete. Rotate the solvent to dryness at 40C, add water (500mL), extract twice with methyl tert-butyl ether (1000mL), combine the extracts, wash with water (300mL), dry with anhydrous sodium sulfate, filter with suction, spin-dry the filtrate, and dry 104.0 g of brown-red solid was obtained, and the two-step yield was 80.0%.
75.9% With 3-chloro-benzenecarboperoxoic acid; In dichloromethane; at 20℃; for 2h; 1 g of 2-aza-non-adamantane obtained in Step 4 was added to 20 ml of dichloromethane,And the addition of m-chloroperoxybenzoic acid 3.5g, stirring at room temperature for 2 hours, TLC controlled analysis,The reaction solution was diluted with saturated sodium bicarbonate 30 ml, extracted twice with 0 ml x 2 dichloromethane, the organic phases were combined,The organic phase was dried with anhydrous potassium carbonate, and the crude product was Nor-AZADO,And purified by column chromatography to give 0.85 g of red solid Nor-AZADO. Yield: 75.9%, GC: 98.5%.
Then, a MeCN solution (14.4 ml) of the crude amine-form, Na2WO4.H2O (0.95 g, 2.88 mmol) was added at room temperature, followed by stirring for 30 minutes. After cooling to 0 C., urea hydrogen peroxide (2.7 g, 28.8 mmol) was added, followed by stirring for 1 hour and then stirring at room temperature for 4 hours. After completion of the reaction was confirmed, H2O (50 ml) was added, followed by extraction with chloroform, and the obtained organic layer was dried over K2CO3. The solvent was removed, and the residue was subjected to column chromatography to obtain ABNO (0.84 g, 6 mmol). The present compound was subjected to mass spectrometry as electron ionized at an accelerating voltage of 3 kV under an ionizing voltage of 70 eV at an ionization current of 300 μA and as a result, a molecular ion peak at m/z 140 and a base peak (100%) at m/z 81 were obtained. Further, characteristic fragment ion peaks at m/z 67, 96, 107 and 122 were obtained.
 

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