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Chemical Structure| 17704-74-4 Chemical Structure| 17704-74-4

Structure of 17704-74-4

Chemical Structure| 17704-74-4

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Product Details of [ 17704-74-4 ]

CAS No. :17704-74-4
Formula : C4H11ClN2O
M.W : 138.60
SMILES Code : CC(C)(N)C(N)=O.[H]Cl
MDL No. :MFCD12913069

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Application In Synthesis of [ 17704-74-4 ]

* 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 [ 17704-74-4 ]

[ 17704-74-4 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 17704-74-4 ]
  • [ 131747-63-2 ]
  • C10H12BrN3O [ No CAS ]
YieldReaction ConditionsOperation in experiment
With sodium acetate; In 1,2-dichloro-ethane; at 20℃; for 18h;Molecular sieve; Description 11 : lambda/2-[(4-Bromo-2-pyridinyl)methyl]-2-methylalaninamide (D11); To a solution of <strong>[131747-63-2]4-bromo-2-pyridinecarbaldehyde</strong> (4 g, 21.5 mmol) (D5) in DCE (160 mL) was added 2-methylalaninamide hydrochloride (D2) (4.47 g, 32.25 mmol),NaOAc (2.65 g, 32.25 mmol) and 4 A molecular sieves (activated in the vacuum oven at 70 0C for 1 day, 20 g) and the resulting mixture was stirred under argon at room temperature. The imine formation was checked by 1H-NMR and after 18 h,NaBH(OAc)3 (6.84 g, 32.25 mmol) and acetic acid (1.94 mL, 32.25 mmol) were added. After stirring for 6 h a NMR sample showed reduction of the imine; saturated aqueous sodium bicarbonate solution (110 mL) was added slowly and the solution was stirred at room temperature for 1 hour after which it was filtered through a pad ofCelite, washed with DCM (100 mL) and the organic layer was separated. The aqueous phase was extracted with DCM (50 mL) and the combined organics were washed with brine (50 mL), dried over MgSO4 and concentrated to afford 5.4 g of <n="33"/>crude material. This was purified by flash chromatography using the Biotage SP4 (40+M silica cartridge), eluting with a gradient of 0 to 10percent MeOH in DCM to yield 5.4 g of the title compound D11.NMR deltaH (CDCI3): 1.43 (6H, s), 1.95 (1 H, broad s), 3.84 (2H, s), 5.36 (1H, broad s), 7.37 (1 H, dd, J = 5.2, 1.6 Hz), 7.47 (1 H, d, J = 1.6 Hz), 7.48 (1 H, broad s), 8.39 (1 H, d, J = 5.2 Hz).LC-MS: MH+ = 272/274, C10H14BrN3O requires 271/273.
 

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