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Resolution of MNR26-1 with (+)-dibenzoyl-D-tartaric acid (MNR5-1)
Hazard and Risk Assessment:
As for MNR2-1
MNR26-5 (MeOH wash fraction) (1.63 g, 6.21 mmol) and MNR5-1 (2.39 g, 6.21 mmol) was dissolved in IPA (13 mL) and water (3 mL) with heating. All the reagents went into solution and the mixture was left to stand and within 15 minutes the mixture was solid. IPA (1mL) was added and with heating the solid broke down into small enough lumps to be filtered. The solid was washed with IPA:water (4:1) and dried to give an off white solid (2.969 g)
The solid was then mixed with IPA (17 mL) and water (3 mL) and heated to reflux. The mixture did not become a solution so IPA (5 mL) and water (2 mL) was added in portions until the refluxing mixture became a solution.
Allowed to cool to room temperature and left in fridge over the weekend. An off white solid had crashed out and was washed with IPA/hexane and dired under vacuum.
Taken to pH 14
Extract EtOAc
Nothing, total crap, just traces
** Reaction not taken any further
Hazard and Risk Assessment:
As for MNR2-1
MNR26-5 (MeOH wash fraction) (1.63 g, 6.21 mmol) and MNR5-1 (2.39 g, 6.21 mmol) was dissolved in IPA (13 mL) and water (3 mL) with heating. All the reagents went into solution and the mixture was left to stand and within 15 minutes the mixture was solid. IPA (1mL) was added and with heating the solid broke down into small enough lumps to be filtered. The solid was washed with IPA:water (4:1) and dried to give an off white solid (2.969 g)
The solid was then mixed with IPA (17 mL) and water (3 mL) and heated to reflux. The mixture did not become a solution so IPA (5 mL) and water (2 mL) was added in portions until the refluxing mixture became a solution.
Allowed to cool to room temperature and left in fridge over the weekend. An off white solid had crashed out and was washed with IPA/hexane and dired under vacuum.
Taken to pH 14
Extract EtOAc
Nothing, total crap, just traces
** Reaction not taken any further