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23rd April 2013 @ 01:09
As for [blog]5901[/blog] [blog]5911[/blog] Starting material from [blog]6847[/blog] Hazard and Risk Assessment:[data]1380[/data] Procedure:MNR11-8 (3.96 g, 10.63 mmol) was dissolved in EtOH (21 mL) and HCl (1M) (110 mL) and heated to reflux for 2.5 hours. The solution was allowed to cool to room temperature then cooled in an ice bath, basified with NaOH pellets (approx 8 g, pellets used to minimise volume of aqueous material) to pH 12-13 and extracted with DCM (4 x 100 mL). The organic fractions were combined, dried over magnesium sulphate, filtered and concentrated under reduced pressure to give an orange crispy solid (1.008 g). TLCReaction mixture after 2.5 hours ran in 100% EtOAc [data]5277[/data] IRĀ [data]5365[/data] Strings Starting material InChI=1S/C21H28N2O4/c1-26-18-10-15-8-9-23-17(16(15)11-19(18)27-2)12-22(13-20(23)24)21(25)14-6-4-3-5-7-14/h10-11,14,17H,3-9,12-13H2,1-2H3 Product InChI=1S/C14H18N2O3/c1-18-12-5-9-3-4-16-11(7-15-8-14(16)17)10(9)6-13(12)19-2/h5-6,11,15H,3-4,7-8H2,1-2H3
Attached Files
mnr26-7 table.PNG
MNR26-3 scheme.png
MNR26-7 scheme.png
2013-04-23 13.15.20.jpg
5f rac IR MNR26-7.jpg