Weekly Report

Solvothermal Experiments

With previous experiments no crystals were observed so again solvothermal reactions were
carried out with different solvent combinations.

A mixture of Bpeb (14.2mg; 0.04mmol) and ZnClO4 (9.3mg; 0.02mmol) dissolved in different
solvent combinations was placed in 5ml glass vial. The vial was sealed and kept at 110oC for
96h, followed by cooling to room temperature for 9 hours. Similar experiments were also done
with ZnNO3 (3.78mg; 0.02mmol).

Reactants Solvent Conditions

DMF (3ml), DMSO(0.5ml)
DMF (3ml), H2O(1ml),DMSO(0.5ml)
DMF (3ml), Ethanol(1ml),DMSO(0.5ml)
DMA (3ml), DMSO(0.5ml)
Bpeb + ZnClO4.6H2O DMA (3ml), H2O(1ml),DMSO(0.5ml)
DMA (3ml), Ethanol(1ml),DMSO(0.5ml)
DME (3ml), DMSO(0.5ml)
DME(3ml), H2O(1ml),DMSO(0.5ml)
DME (3ml), Ethanol(1ml),DMSO(0.5ml)
DMF (3ml), DMSO(0.5ml)
DMF (3ml), H2O(1ml),DMSO(0.5ml)
DMF (3ml), Ethanol(1ml),DMSO(0.5ml)
DMA (3ml), DMSO(0.5ml)
Bpeb + ZnNO3 DMA (3ml), H2O(1ml),DMSO(0.5ml)
DMA (3ml), Ethanol(1ml),DMSO(0.5ml)
DME (3ml), DMSO(0.5ml)
DME(3ml), H2O(1ml),DMSO(0.5ml)
DME (3ml), Ethanol(1ml),DMSO(0.5ml)

Layering Experiments

No crystals were observed with DMF solvent. So layering experiment was conducted with
DMSO as it showed better dissolution. Three experiments were conducted using same
conditions. DCM in combination with DMSO, ethanol in combination with DMSO, DMA and
DME were also tried to check dissolution of BPEB but it poorly dissolved in the mentioned
solvents.
0.03mmol 0.03mmol 0.03mmol 0.03mmol
ZnClO4 in ZnClO4 ZnClO4 ZnClO4
methanol in acetone in methanol in acetone

Buffer Buffer Buffer

Buffer
0.06mmol 0.06mmol 0.06mmol 0.06mmol
Bpeb in Bpeb in Bpeb in Bpeb in
DMF/DMSO DMF/DMSO DMF/DMSO DMF/DMSO
+ acid + acid

0.03mmol 0.03mmol 0.03mmol 0.03mmol

AgClO4 AgClO4 AgClO4 AgClO4
in methanol in acetone in methanol in acetone
Buffer Buffer
Buffer Buffer
0.06mmol 0.06mmol
0.06mmol 0.06mmol Bpeb in
Bpeb in Bpeb in Bpeb in
DMF/DMSO DMF/DMSO
DMF/DMSO DMF/DMSO + acid +acid

0.03mmol 0.03mmol 0.03mmol 0.03mmol

CdNO3 CdNO3 CdNO3 CdNO3
in methanol in acetone in methanol in acetone
Buffer Buffer
Buffer Buffer
0.06mmol 0.06mmol
0.06mmol 0.06mmol Bpeb in Bpeb in
Bpeb in Bpeb in DMF/DMSO DMF/DMSO
DMF/DMSO DMF/DMSO + acid +acid