sulfuric acid T=125°C; 2 h; Title compound not separated from byproducts;

sulfuric acid T=20 - 125°C; 2 h;

1.1: dihydrogen peroxide; acetic acid / water / 70 °C 2.1: water / 4 h / 20 - 100 °C 3.1: sulfuric acid / 20 - 130 °C 3.2: Cooling with ice View Scheme

1: 94 percent / 30percent H2O2 / acetic acid / 12 h / 75 °C 2: 77 percent / 3.5 h / 100 °C 3: conc. H2SO4 / 2 h / 125 °C View Scheme

1.1: water / 4 h / 20 - 100 °C 2.1: sulfuric acid / 20 - 130 °C 2.2: Cooling with ice View Scheme

1: 77 percent / 3.5 h / 100 °C 2: conc. H2SO4 / 2 h / 125 °C View Scheme

potassium in tetrahydrofuran; toluene byproducts: KPF6, KBr, H2; N2-atmosphere; dropwise addn. of org. compd. in THF to K in toluene, refluxing (2 h), cooling to room temp., dropwise addn. of Mn-complex in THF, stirring (room temp., overnight); solvent removal (vac.), addn. of CH2Cl2, filtration, solvent removal (vac.), addn. of pentane, chromy. (Al2O3, pentane, then CH2Cl2/pentane=1:7);