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Chemical Structure| 117007-77-9 Chemical Structure| 117007-77-9

Structure of 117007-77-9

Chemical Structure| 117007-77-9

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Product Details of [ 117007-77-9 ]

CAS No. :117007-77-9
Formula : C5H5ClN2O
M.W : 144.56
SMILES Code : O=CC1=C(Cl)N(C)N=C1
MDL No. :MFCD16619816
InChI Key :BRTDPKPJDXNQEX-UHFFFAOYSA-N
Pubchem ID :15145019

Safety of [ 117007-77-9 ]

GHS Pictogram:
Signal Word:Warning
Hazard Statements:H315-H319-H335
Precautionary Statements:P261-P264-P271-P280-P302+P352-P304+P340-P305+P351+P338-P312-P332+P313-P337+P313-P362-P403+P233-P405-P501

Application In Synthesis of [ 117007-77-9 ]

* 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 [ 117007-77-9 ]

[ 117007-77-9 ] Synthesis Path-Downstream   1~2

  • 1
  • [ 68-12-2 ]
  • [ 10234-66-9 ]
  • [ 117007-77-9 ]
  • 2
  • [ 34846-90-7 ]
  • [ 68-12-2 ]
  • [ 60-34-4 ]
  • [ 117007-77-9 ]
YieldReaction ConditionsOperation in experiment
52% [0170] A magnetically stirred solution of methyl 3-methoxyacrylate (20.0 g, 172.2 mmol) in methanol (100 mL) was treated slowly with N-methylhydrazine (10.0 mL, 189.4 mmol) then heated at reflux for 16 hours. The resulting mixture was cooled to room temperature then concentrated under reduced pressure to afford an orange solid that was dissolved in N,N-Dimethyformamide (DMF) (19.9 mL, 258.4 mmol) and cooled to 0 °C. The resulting mixture was treated slowly with phosphoryl chloride (48.1 mL, 516.6 mmol) then heated at 80 °C for 7 hours before being cooled and poured slowly into ice cold Na2C03 (600 mL of a 20percent w/v aqueous solution). The aqueous solution was then extracted with chloroform (5 x 100 mL) and the combined organic phases were washed with brine (1 x 100 mL) before being dried (MgS04), filtered and concentrated under reduced pressure to afford an orange solid. Recrystallisation (dichloromethane/hexane) afforded compound 1 (12.87 g, 52percent) as yellow crystals, m.p. 77-78 °C, (R = 0.44 in 1: 1 v/v ethyl acetate/hexane).
 

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