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27th November 2013 @ 10:54

Methyl 2-pyrazinecarboxylate (5.10 g) was suspended in 1,2 - dichloroethane (50.80 ml) and mCPBA (16.43 g) was added. The reaction was stirred at 60 oC for 18 hours. The reaction was allowed to cool to room tmperature sand diluted with CH2Cl2 (152 ml). The percipitate was filtered off and washed with additional CH2Cl2 (3 x 17.80 ml). The filtrate was combines, dried over K2CO3, filtered and concentrated under vacuum. The residue was suspended in hexane (25.40 ml). the product was isolated using filtration, washed with additional hexane (2 x 25.40 ml) to afford a light yellow solid (9.46 g) 1H NMR was dervived (EO 5-2A 1H NMR) NMR showed m-CPBA present so sample was purified.

Solid was washed with addition of Et2OAc (250 ml) which was then wahsed with NaHCO3 (250 ml). This wash was done three times and TLC'ed against product (EO 5-1) in 5% Et2OAc in DCM (EO TLC 5-2A) TLC showed that product was still present in the aqueous layer so three additional washes of the aqueous layer was carried out with DCM (250 ml) and methanol (50 ml) TLC was taken (EO TLC 5-2B). TLC showed most of the product had left aquous layer so all the collected organic layers were collected and solvent was removed under pressure to give a solid (5.08 g) (xxxd yield) NMR of the purified solid was derived (EO 5-2B 1H NMR).

 

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Attached Files
EO 5-2A 1H NMR.pdf
risk assesment EO 5-2.doc
EO 5-2A 3ORProject9_EO5-2A_261113_1H_dl400.tar
EO 5-2B 1H NMR.pdf
EO TLC 5-2A.jpeg
EO TLC 5-2B.jpeg
Reaction scheme EO 5-1 new.jpg