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Chemical Structure| 861046-07-3 Chemical Structure| 861046-07-3

Structure of 861046-07-3

Chemical Structure| 861046-07-3

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Product Details of [ 861046-07-3 ]

CAS No. :861046-07-3
Formula : C9H12N2
M.W : 148.21
SMILES Code : CC1NC2=C(C=CC=N2)CC1

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Application In Synthesis of [ 861046-07-3 ]

* 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 [ 861046-07-3 ]

[ 861046-07-3 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 1569-16-0 ]
  • [ 861046-07-3 ]
  • [ 274676-47-0 ]
YieldReaction ConditionsOperation in experiment
With palladium 10% on activated carbon; hydrogen; In methanol; at 25℃; under 3102.97 Torr; for 23h;Inert atmosphere; To a mixture of 10percent palladium on carbon (0.369 g, 0.347 mmol) in MeOH (20 mL) under nitrogen in a 500 mL Parr reaction vessel was added 2-methyl-l,8-naphthyridine (0.500 g, 3.47 mmol). The reaction mixture was vacuum flushed with nitrogen (3x), then with hydrogen (3x) and vigorously shaken under hydrogen at 60 psi at -25 °C for 23 h. The reaction was filtered through a pad of Celite and thoroughly washed with MeOH. The filtrated was concentrated in vacuo to afford a mixture of the title compounds (506.1 mg) as a white solid. NMR indicated a mixture of two products in a ratio of 1 :0.18 which was used without further purification. LC-MS retention time = 1.70 min; m/z = (0434) 149.06 [M+H]+. (Column: Phenomenex Luna CI 8 50 x 2.0 mm 3 muiotaeta. Solvent A = 90percent Water : 10percent MeOH : 0.1percent TFA. Solvent B = 10percent Water : 90percent MeOH : 0.1percent TFA. Flow Rate = 0.8 mL/min. Start percent B = 0. Final percent B = 100. Gradient Time = 4 minutes, then a 1 minute hold at 100percent B. Oven temperature = 40 °C. Wavelength = 220 nm). Major product: NMR (400 MHz, DMSO-d6) delta 6.99 (d, J=7.3 Hz, 1H), 6.24 (d, J=7.0 Hz, 1H), 6.21 (br s, 1H), 3.26 - 3.19 (m, 2H), 2.59 (t, J=6.3 Hz, 2H), 2.16 (s, 3H), 1.74 (dt, J=l 1.7, 6.0 Hz, 2H). Minor product: NMR (400 MHz, DMSO-d6) delta 7.76 - 7.69 (m, 1H), 7.12 (d, J=7.0 Hz, 1H), 6.39 (dd, J=7.2, 4.9 Hz, 1H), 3.49 - 3.33 (m, 1H), 2.70 - 2.61 (m, 2H), 1.89 - 1.78 (m, 1H), 1.47 - 1.33 (m, 1H), 1.15 (d, J=6.3 Hz, 3H).
 

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