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13th July 2017 @ 05:42

Summary

Synthesis of precursor towards the "the Alkyl" - see GHI#508

 

References

Synthesis of 2-Chloro-6-hydrazinylpyrazine (AEW 85-x)

 

Reaction Scheme

Synthesis of blah from blah

Procedure

Compound mol. wt. quantity d (liq.) n (mmol) equiv.
2,6-dichloropyrazine 148.98 2.30 g   15.4 mmol 1
hydrazine hydrate 50.06 1.5 mL 1.029 30.8 mmol 2
           
           
           

Hydrazine hydrate (1.5 mL) was added to a stirred soilution of 2,6-dichloropyrazine in EtOH (30 mL). The reaction mixture was heated to reflux then maintained at this temperature for 3 hours. The mixture was cooled to rt, then solvent was removed under reduced pressure.

The resultant solid was dissolved in EtOAc (25 mL) and water (25 mL) was added. The layers were separated and the aqueous phase was extracted with EtOAc (3 x 10 mL). The combined organic layers were washed with brine and dried with MgSO4 before being concentrated under reduced pressure to yield the final product as a biege solid.

 

Risk assessment

Risk Assesment form.pdf

 

Data

{pic of reaction TLC}

 

1H NMR:

Sample 1H NMR.pdf
 
Sample_NMR.zip

 

Compound Strings

InChIKey=LSEAAPGIZCDEEH-UHFFFAOYSA-N

to

InChIKey=FEDQSVIJHNBUHH-UHFFFAOYSA-N

 

InChI=1S/C4H2Cl2N2/c5-3-1-7-2-4(6)8-3/h1-2H

to

InChI=1S/C4H5ClN4/c5-3-1-7-2-4(8-3)9-6/h1-2H,6H2,(H,8,9)

 

ClC1=CN=CC(Cl)=N1

to

NNC1=NC(Cl)=CN=C1

Attached Files
sample_scheme.png
Risk Assesment form.pdf
Sample 1H NMR.pdf
Sample_NMR.zip
Comments
Re: Synthesis of [COMPOUND NAME] by Mark Coster
13th July 2017 @ 13:24
Please note this entry was created as part of a tutorial - it's not a real experimental procedure!