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Chemical Structure| 823189-69-1 Chemical Structure| 823189-69-1

Structure of 823189-69-1

Chemical Structure| 823189-69-1

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Product Details of [ 823189-69-1 ]

CAS No. :823189-69-1
Formula : C7H9N3O2
M.W : 167.17
SMILES Code : O=C(C1=CC=NN=C1)N(OC)C

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Application In Synthesis of [ 823189-69-1 ]

* 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.

  • Upstream synthesis route of [ 823189-69-1 ]

[ 823189-69-1 ] Synthesis Path-Upstream   1~1

  • 1
  • [ 823189-69-1 ]
  • [ 75-16-1 ]
  • [ 50901-46-7 ]
YieldReaction ConditionsOperation in experiment
42%
Stage #1: at 0℃; for 1 h;
Stage #2: With water; sodium chloride In tetrahydrofuran; diethyl ether
To N-methoxy-N-methylpyridazine-4-carboxamide (1.13 g, 6.76 mmol) in tetrahydrofuran (22 mL) , methylmagnesium bromide (10.1 mL, 10.1 mmol, IM in diethyl ether) was added dropwise at 0°C in a nitrogen stream, and the resulting solution was stirred for 1 hour. After completion of the reaction, the reaction solution was mixed with saturated aqueous sodium chloride and <n="130"/>extracted with chloroform, and the extract was dried over anhydrous sodium sulfate and evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography (hexane/ethyl acetate= 1/2 --> 0/1) to give the desired product (42percent yield) . Morphology: pale yellow solid LC/MS: Condition 7, retention time 0.75 min LC/MS (ESI+) m/z; 123 [MH-I] + 1H-NMR(CDCl3) δ :2.70 (s, 3H), 7.86 (dd, J = 0.8 and 5.4 Hz, 1H), 9.48 (d, J = 5.4 Hz, 1H), 9.61 (d, J = 0.8 Hz, 1H)
References: [1] Patent: WO2009/57827, 2009, A1, . Location in patent: Page/Page column 127-128.
 

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