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Step 1: tert-butyl 2-amino-3-methylbutanoateTo a stirred solution of DL- valine (25 g, 0.213 mol) in tert-butyl acetate (250 mL) at 0C, was added HCI04 (64.2 g, 0.320 mol) portionwise. The reaction mixture was stirred for 36 h at RT. It was diluted with water and extracted in ethyl acetate (500 mL). The organic layer was washed with a 10% sodium bicarbonate solution (2x150 mL), dried over Na2S04 and concentrated, affording of the title compound as brown liquid. 1H NMR (DMSO-d6, 400 MHz) δ 7.31 (brs, 2H), 3.62(d, J = 4.4 Hz, 1 H), 1 .98 (d, J = 1.7 Hz, 1 H), 1.44(s, 9H), 0.95 (m, 6H).
General procedure: The metal chlorides of Fe(III), Co(II), Ni(II), Cu(II),Mn(II), Cr(III) andZn(II) solutions (1 mmol) in bidistilled water (25 mL) were added to25 mL ethanol solution of H2Ten (0.337 g, 1mmol) followed by additionof 25 mL of 1 mmol Val (0.117 g in bidistilled water) in the molar ratio1:1:1 (metal salt: H2Ten: Val) in total volume 75 mL mixture. Theresulting mixture was stirred under reflux for 2 h whereupon the complexes precipitated. They were removed by filtration, washed withhot ethanol followed by diethylether and dried in vacuum desiccatorsover anhydrous calcium chloride
General procedure: The metal chlorides of Fe(III), Co(II), Ni(II), Cu(II),Mn(II), Cr(III) andZn(II) solutions (1 mmol) in bidistilled water (25 mL) were added to25 mL ethanol solution of H2Ten (0.337 g, 1mmol) followed by additionof 25 mL of 1 mmol Val (0.117 g in bidistilled water) in the molar ratio1:1:1 (metal salt: H2Ten: Val) in total volume 75 mL mixture. Theresulting mixture was stirred under reflux for 2 h whereupon the complexes precipitated. They were removed by filtration, washed withhot ethanol followed by diethylether and dried in vacuum desiccatorsover anhydrous calcium chloride
General procedure: The metal chlorides of Fe(III), Co(II), Ni(II), Cu(II),Mn(II), Cr(III) andZn(II) solutions (1 mmol) in bidistilled water (25 mL) were added to25 mL ethanol solution of H2Ten (0.337 g, 1mmol) followed by additionof 25 mL of 1 mmol Val (0.117 g in bidistilled water) in the molar ratio1:1:1 (metal salt: H2Ten: Val) in total volume 75 mL mixture. Theresulting mixture was stirred under reflux for 2 h whereupon the complexes precipitated. They were removed by filtration, washed withhot ethanol followed by diethylether and dried in vacuum desiccatorsover anhydrous calcium chloride
General procedure: The metal chlorides of Fe(III), Co(II), Ni(II), Cu(II),Mn(II), Cr(III) andZn(II) solutions (1 mmol) in bidistilled water (25 mL) were added to25 mL ethanol solution of H2Ten (0.337 g, 1mmol) followed by additionof 25 mL of 1 mmol Val (0.117 g in bidistilled water) in the molar ratio1:1:1 (metal salt: H2Ten: Val) in total volume 75 mL mixture. Theresulting mixture was stirred under reflux for 2 h whereupon the complexes precipitated. They were removed by filtration, washed withhot ethanol followed by diethylether and dried in vacuum desiccatorsover anhydrous calcium chloride
General procedure: The metal chlorides of Fe(III), Co(II), Ni(II), Cu(II),Mn(II), Cr(III) andZn(II) solutions (1 mmol) in bidistilled water (25 mL) were added to25 mL ethanol solution of H2Ten (0.337 g, 1mmol) followed by additionof 25 mL of 1 mmol Val (0.117 g in bidistilled water) in the molar ratio1:1:1 (metal salt: H2Ten: Val) in total volume 75 mL mixture. Theresulting mixture was stirred under reflux for 2 h whereupon the complexes precipitated. They were removed by filtration, washed withhot ethanol followed by diethylether and dried in vacuum desiccatorsover anhydrous calcium chloride
General procedure: The metal chlorides of Fe(III), Co(II), Ni(II), Cu(II),Mn(II), Cr(III) andZn(II) solutions (1 mmol) in bidistilled water (25 mL) were added to25 mL ethanol solution of H2Ten (0.337 g, 1mmol) followed by additionof 25 mL of 1 mmol Val (0.117 g in bidistilled water) in the molar ratio1:1:1 (metal salt: H2Ten: Val) in total volume 75 mL mixture. Theresulting mixture was stirred under reflux for 2 h whereupon the complexes precipitated. They were removed by filtration, washed withhot ethanol followed by diethylether and dried in vacuum desiccatorsover anhydrous calcium chloride
General procedure: The metal chlorides of Fe(III), Co(II), Ni(II), Cu(II),Mn(II), Cr(III) andZn(II) solutions (1 mmol) in bidistilled water (25 mL) were added to25 mL ethanol solution of H2Ten (0.337 g, 1mmol) followed by additionof 25 mL of 1 mmol Val (0.117 g in bidistilled water) in the molar ratio1:1:1 (metal salt: H2Ten: Val) in total volume 75 mL mixture. Theresulting mixture was stirred under reflux for 2 h whereupon the complexes precipitated. They were removed by filtration, washed withhot ethanol followed by diethylether and dried in vacuum desiccatorsover anhydrous calcium chloride
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