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21st February 2012 @ 07:02
Screening conditions for optimum resolution of MNR26-1 with (-)-dibenzoyl-L-tartaric acid (MNR6-1) to obtain R-di-methoxy-PZQamine (MNR27-x)

* As a result of mnr27-1 not working.

MNR27-1%20scheme.png

mnr27-1%20table.PNG

Hazard and Risk Assessment:
As for MNR2-1

MNR27-2

MNR26-1 (0.08 g, 0.3 mmol) and (-)-dibenzoyl-L-tartaric acid. 2IPA (0.15 g, 0.3 mmol) was dissolved in isopropanol (4 mL) in a vial and heated with the heat gun to dissolve the reagents.

Everything went into solution and the vial was left to stand at room temperature overnight.

Some material crashed out and was filtered with hexane to give brown crystals/solid. 12 mg


MNR27-3

MNR26-1 (0.08 g, 0.3 mmol) and (-)-dibenzoyl-L-tartaric acid. 2IPA (0.15 g, 0.3 mmol) was dissolved in hexane (4 mL) in a vial and heated with the heat gun to dissolve the reagents.

very little went into solution and the vial was left to stand at room temperature overnight.

As little went into solution this was not taken any further

MNR27-4

MNR26-1 (0.08 g, 0.3 mmol) and (-)-dibenzoyl-L-tartaric acid. 2IPA (0.15 g, 0.3 mmol) was dissolved in IPA (1 mL) ans hexane(3 mL) in a vial and heated with the heat gun to dissolve the reagents.

very little went into solution and the vial was left to stand at room temperature overnight.

As little went into solution this was not taken any further

MNR27-5

MNR26-1 (0.08 g, 0.3 mmol) and (-)-dibenzoyl-L-tartaric acid. 2IPA (0.15 g, 0.3 mmol) was dissolved in IPA (2 mL) ans hexane(2 mL) in a vial and heated with the heat gun to dissolve the reagents.

some went into solution but not completely, the vial was left to stand at room temperature overnight.

The sample looked very meesy in the morning and was not taken any further

MNR27-6

MNR26-1 (0.08 g, 0.3 mmol) and (-)-dibenzoyl-L-tartaric acid. 2IPA (0.15 g, 0.3 mmol) was dissolved in IPA (3 mL) ans hexane(1 mL) in a vial and heated with the heat gun to dissolve the reagents.

everything went into solution and the vial was left to stand at room temperature overnight.

Some material crashed out and was filtered with hexane to give brown crystals/solid. 20 mg

MNR27-7

MNR26-1 (0.08 g, 0.3 mmol) and (-)-dibenzoyl-L-tartaric acid. 2IPA (0.15 g, 0.3 mmol) was dissolved in IPA (3.8 mL) ans water(0.2 mL) in a vial and heated with the heat gun to dissolve the reagents.

everything went into solution and the vial was left to stand at room temperature overnight.

Some material crashed out and was filtered with hexane to give brown crystals/solid. 85 mg

MNR27-8

MNR26-1 (0.08 g, 0.3 mmol) and (-)-dibenzoyl-L-tartaric acid. 2IPA (0.15 g, 0.3 mmol) was dissolved in IPA (4 mL) ans hexane (4 mL) in a vial and heated with the heat gun to dissolve the reagents.

some went into solution but not completely, the vial was left to stand at room temperature overnight.

The sample looked very messy and was not taken any further

MNR27-9

MNR26-1 (0.08 g, 0.3 mmol) and (-)-dibenzoyl-L-tartaric acid. 2IPA (0.15 g, 0.3 mmol) was dissolved in DCM (2 mL) ans hexane (2 mL) in a vial and heated with the heat gun to dissolve the reagents.

some went into solution but not completely, the vial was left to stand at room temperature overnight.

The sample completely congealed overnight and was not taken any further

MNR27-10

MNR26-1 (0.08 g, 0.3 mmol) and (-)-dibenzoyl-L-tartaric acid. 2IPA (0.15 g, 0.3 mmol) was dissolved in DCM (2 mL) ans IPA(2 mL) in a vial and heated with the heat gun to dissolve the reagents.

everything went into solution but not completely, the vial was left to stand at room temperature overnight.

Hexane was added and material crashed out and was filtered with hexane to give light brown crystals/solid. 121 mg

MNR27-11

MNR26-1 (0.08 g, 0.3 mmol) and (-)-dibenzoyl-L-tartaric acid. 2IPA (0.15 g, 0.3 mmol) was dissolved in DCM (1 mL) ans IPA(3 mL) in a vial and heated with the heat gun to dissolve the reagents.

everything went into solution but not completely, the vial was left to stand at room temperature overnight.

Hexane was added and material crashed out and was filtered with hexane to give brown crystals/solid. 118 mg
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