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11th September 2016 @ 14:32

(started on 9/8)

Link to last attempt: Synthesis of 2-Chloro-6-hydrazinylpyrazine (MRLS 1-1). This time we are using more starting material for use in both continuation of the Nemesis synthesis outlined here and for synthesis of the triazolopyrazine core.

 

first step of nemesis synthesis

compound

MW (g/mol)

mol (mmol) g           density (g/mL) volume (mL) equivalents
[2,6] dichloropyrazine 148.98 13.4 2     1
hydrazine hydrate 32.045 13.4 0.680   0.66 1
ethanol         20  
2-Chloro-6-hydrazinylpyrazine 144.56  13.4  1.937     1

 

[2,6]-Dichloropyrazine (2 g, 13.4 mmol) was stirred in ethanol (10 mL) and hydrazine hydrate (80% by volume, 0.83 mL). The mixture was refluxed at 80 ˚C  under Ar for ~24 hours. 

(9/9)

The resulting mixture was vacuum filtered to yield a crude white/yellow solid.

The remaining solvent was removed under reduced pressure to give an orange solid (1.0906 g, 56% yield). 

Attached Files
MRLS 1-2.pdf.lnk
MRLS 1-2.pdf