All Notebooks | Help | Support | About
6th November 2017 @ 15:18

Step 2 .jpg

Masses and measurements:

Hydrazone - 1.5054g, 4.84mmol

BAIB - 1.7038g, 5.29mmol

Dichloromethane - 30mL

Procedure:

The hydrazone product (1.5054g, 4.84mmol) was dissolved in a RBF using dichloromethane (30mL) whilst being stirred. Once the solid was fully dissolved, BAIB (1.7038g, 5.29mmol) was added to the reaction mixture  and the mixture was left to stir for 2-3 hours. The reaction mixture was a thick cloudy orange mixture and continued to look the same until the end of the reaction. Next the reaction was quenched by adding NaHCO3 (30mL) and the remaining solution was extracted and seperated using ethyl acetate (3x40mL). Next the retained organic layers were dried with MgSO4 and the precipitate was filtered out leaving behind the filtrate of organic layers which was subsequently rotary evaporated leaving behind an orange solid. The remaining solid was then seperated on a flash column (1:1 ethyl acetate & pet ether) where it was found that test tubes 1-17 contained the end product; these test tubes were combined, rotary evaporated and the product of 3-(4-bromophenyl)-5-chloro-[1,2,4]triazolo[4,3,a]pyrazine (0.5854g, 39.13%) was formed as a pale orange crystal like solid. 

step 22.jpg

step 2.jpg
Attached Files
Step 2 .jpg
step 2.jpg
step 22.jpg