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12th October 2011 @ 07:25
Attempts to improve promising results of MW56-3

MNR11-4%20scheme.png

MNR11-4%20table.PNG

Hazard and Risk Assessment:
As for MNR11-3

Procedure

MNR11-4
MNR8-2(50 mg, 0.11 mmol) and 1,1’-Binaphthalene-2,2’-disulfonic acid, MW54-3 (10 mg, 0.01 mmol) DCM (1 mL) was heated at reflux overnight

MNR11-5
MNR8-2(50 mg, 0.11 mmol) and 1,1’-Binaphthalene-2,2’-disulfonic acid, MW54-3 (10 mg, 0.01 mmol) chloroform (1 mL) was heated at reflux overnight

MNR11-6
MNR8-2(50 mg, 0.11 mmol) and 1,1’-Binaphthalene-2,2’-disulfonic acid, MW54-3 (10 mg, 0.01 mmol) DCM (1 mL) was stirred at room temperature overnight

MNR11-7
MNR8-2(50 mg, 0.11 mmol) and 1,1’-Binaphthalene-2,2’-disulfonic acid, MW54-3 (10 mg, 0.01 mmol) chloroform (1 mL) was stirred at room temperature overnight

MNR11-8
MNR8-2(100 mg, 0.22 mmol) and 1,1’-Binaphthalene-2,2’-disulfonic acid, MW54-3 (20 mg, 0.02 mmol) toluene (2 mL) was stirred at room temperature overnight

TLC of all 5 reactions after 16 hours showed very little reaction. MNR11-5 (refluxing chloroform) showed signs of possible product. After 20 hours a sample of MNR11-5 was removed from the reaction and filtered through a pipette of silica and ran through the LCMS.

All 5 reactions were left at their original temperatures for XX hours.
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Attached Files
MNR11-4 table.PNG
MNR11-4 scheme.png