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30th September 2016 @ 04:23

(started on 9/28)

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 26.8 4     1
hydrazine hydrate 32.045 26.8 0.88   1.78 1
ethanol         40  
2-Chloro-6-hydrazinylpyrazine 144.56  26.8  3.95g      1

 

[2,6]-Dichloropyrazine (4 g, 26.8 mmol) was stirred in ethanol (40 mL) and hydrazine hydrate (80% by volume, 1.78 mL). The mixture was refluxed at 80 ˚C  under Ar for ~24 hours. 

(9/29)

Solvent removed under reduced pressure. Resulting yellow solid dissolved in 30mL water and 40mL ethyl acetate. aqueous layer extracted 3x20mL etoac. combined organic layers washed with 20 mL brine, and then organic layer removed under reduced pressure. yield of 3.60g, 24.9mmol, 92% yield.