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Chemical Structure| 133261-06-0 Chemical Structure| 133261-06-0

Structure of 133261-06-0

Chemical Structure| 133261-06-0

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Product Details of [ 133261-06-0 ]

CAS No. :133261-06-0
Formula : C9H12N2O2
M.W : 180.20
SMILES Code : O=C(C1=NNC(C2CC2)=C1)OCC
MDL No. :MFCD08277218

Safety of [ 133261-06-0 ]

GHS Pictogram:
Signal Word:Warning
Hazard Statements:H302-H315-H319-H335
Precautionary Statements:P261-P305+P351+P338

Application In Synthesis of [ 133261-06-0 ]

* 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 [ 133261-06-0 ]

[ 133261-06-0 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 21080-80-8 ]
  • [ 133261-06-0 ]
YieldReaction ConditionsOperation in experiment
With hydrazine hydrate; acetic acid; In tetrahydrofuran;Reflux; General procedure: To a mixture of t-BuOK (92.0 g, 697 mmol) and THF (500 mL) was added a mixture of 3-methyl-2-butanone (50.0 g, 581 mmol) and diethyl oxalate (85.8 g, 587 mmol) dropwise over 1 h. The mixture was stirred at room temperature for 15 h to form ethyl 5-methyl-2,4-dioxohexanoate. Thereafter, AcOH (80 mL, 1.39 mol) and hydrazine hydrate (32.0 g, 639 mmol) were successively added. The mixture was heated under reflux with stirring for 2 h. After being cooled, the mixture was concentrated in vacuo and the residue was partitioned between EtOAc and water. The organic solution was washed with sat. NaHCO3 and brine, dried over MgSO4, and concentrated under reduced pressure. The residue was purified by silica gel chromatography (hexane/EtOAc, 9:1 to 1:1) to give 20a (57.7 g, 55percent) as a brown oil.
 

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