复旦大学：《有机化学实验 Organic chemistry lab》课程教学资源（实验讲义）Preparation of Manganese（III）Acetyllacetonate

Organic Chemistry Experiments Preparation of manganese(lD) acetylacetonate 三画日

Preparation of Manganese(III) Acetyllacetonate Organic Chemistry Experiments

E Purposes and requirements Complex or coordination compound, a class of substances in which a central metal atom is surrounded by other nonmetal atoms. through the preparation of manganese(lll) acetylacetonate, you can be familiar with the following knowledge 1. Master the synthetic methods of complexes 2. Master the operation of mixed solvent recrystallization 3. Review the manipulations of reflux and simple distillation reaction device

Purposes and requirements 1. Master the synthetic methods of complexes 2. Master the operation of mixed solvent recrystallization 3. Review the manipulations of reflux and simple distillation reaction device Complex or Coordination compound, a class of substances in which a central metal atom is surrounded by other nonmetal atoms. Through the preparation of manganese(III) acetyllacetonate, you can be familiar with the following knowledge:

2 Principle CH3 KMno 4 H2 H3C KMnOa undergoes a redox reaction with acetylacetone Mn vll is reduced to Mn!ll and then coordinated with acetylacetone to afford manganese(lIn) acetylacetonate

Principle KMnO4 undergoes a redox reaction with acetylacetone, MnVII is reduced to MnIII , and then coordinated with acetylacetone to afford manganese(III) acetyllacetonate

2 Reagents Acetylacetone: CH3 COCH3 F.W.100. 11 b.p.1399C d.0.976 Potassium permanganate: KMnO4 FW.159.00 Acetone: CH COCH FW.5808 bp.56 d.0.788 Petroleum ether: b p 60-90 oC Manganese(llD acetylacetonate: Mn(CSH,O2)3 bp.60-90C

Reagents Acetylacetone: CH3COCH2COCH3 F.W. 100.11 b.p. 139 oC d. 0.976 Potassium permanganate: KMnO4 F.W. 159.00 Acetone: CH3COCH3 F.W. 58.08 b.p. 56 oC d. 0.788 Petroleum ether: b.p. 60-90 oC Manganese(III) acetyllacetonate: Mn(C5H7O2 )3 b.p. 60-90 oC

2 Procedures 1)KMnO4(1 g)+ H2,O(10 mL), stirred at 75oC; 2)Add acetylacetone 4.4 g(4. 8 mL) dropwise and stir at 75 oC for 10 min 3)Remove heating, cooled with ice-water bath for 10 min 4)Filtered, washed with H,O and 30% Etoh, then dried to constant weight 5)Recrystallization with acetone-petroleum ether ow-.j

Procedures 1）KMnO4 (1 g) + H2O (10 mL), stirred at 75 oC; 2）Add acetylacetone 4.4 g (~ 4.8 mL) dropwise and stir at 75 oC for 10 min; 3）Remove heating, cooled with ice-water bath for 10 min ； 4）Filtered, washed with H2O and 30% EtOH, then dried to constant weight; 5） Recrystallization with acetone-petroleum ether

NIV 2 Procedures 9 Apparatus for preparation ◆ Recrystallization

Procedures  Apparatus for preparation  Recrystallization

2 Procedures preparation ◆ Filtered and washe ◆ Recrystallization ◆ Dried under ir

Procedures  preparation  Filtered and washed  Recrystallization  Dried under IR

月 Notes The reaction is very violent when initiating. Therefore, acety lactone needs to be added dropwise 2) The product has good solubility in ethanol. So the the concentration of EtoH should not be too high during washing 》

Notes 1) The reaction is very violent when initiating. Therefore, acetylacetone needs to be added dropwise. 2) The product has good solubility in ethanol. So the the concentration of EtOH should not be too high during washing