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1st November 2017 @ 13:45

VTM005

23/10/2017

VTM005.jpg

VTM004 (0.037 g, 0.08 mmol) was dissolved in toluene (2 mL). Pyrrolidine (0.007 g, 0.96 mmol), NaO t Bu (0.011 g, 0.11 mmol), BINAP (0.37 mg, 0.6 µmol) and Pd 2 (dpa) 3 (0.7 mg, 0.8 µmol) were added in this order to the solution and the mixture was heated at 80 °C for 16 hours. TLC analysis showed the presence of large quantities of the starting material.

VTM005 TLC 16hours.jpg

The temperature was increased to 100 °C and the reaction left to stir for two weeks. NMR analysis showed no formation of the final product.

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10th October 2017 @ 12:27

VTM001.jpg

 

3,4-difluorophenyl acetic acid was mixed with 1M LiAlH 4 in THF (6.3 mL, 6.3 mmol) at 0°C and stirred for 24 hours. It was then heated to reflux for an hour and cooled down to room temperature. The mixture was treated with 2M HCl (40 mL) and EtOAc (40mL). The organic layer was extracted (2 x 20mL EtOAc) and concentrated in vacuo. The crude was obtained as a pale yellow oil and purified via column chromatography (Petroleum Ether 1:1 EtOAc) to yield clear liquid as a final product (0.3 g, 33 %)

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