dipotassium hydrogenphosphate; .alpha.,.alpha.,.alpha.-trichloroacetamide; dihydrogen peroxide in dichloromethane; water T=20 - 31°C; 7.5 - 12.6 h; Product distribution / selectivity;

dipotassium hydrogenphosphate; dihydrogen peroxide

1: 20.25 h; Heating / reflux; 2: With hydrogenchloride in methanol; water Heating / reflux; 3: With dipotassium hydrogenphosphate; formic acid; dihydrogen peroxide; potassium formiate; acetic anhydride; methanesulfonyl chloride; triethylamine; trichloroacetonitrile more than 3 stages;

1.1: potassium carbonate; dimethyloctadecylbenzylammonium chloride / N,N-dimethyl-formamide / 48 h / 90 °C 2.1: acetic acid / N,N-dimethyl-formamide / 0.5 h / 45 °C 2.2: 4 h 3.1: potassium carbonate / 0 - 20 °C 4.1: triethylamine / dichloromethane / 0 °C 5.1: potassium formiate; formic acid / acetic anhydride / 100 °C 6.1: .alpha.,.alpha.,.alpha.-trichloroacetamide; dihydrogen peroxide; dipotassium hydrogenphosphate / dichloromethane / 10 - 20 °C View Scheme

1: 82 g / AlEt3 / hexane; tetrahydrofuran / 0.5 h / Heating 2: 6.9 g / DIBAH / 1,2-dimethoxy-ethane; hexane / 2 h / 5 °C 3: 6.6 g / aq. CrO3, H2SO4 / acetone / 0.5 h / 5 °C 4: 2.7 g / CH2Cl2; diethyl ether / 0.17 h 5: 71.6 percent / aq. H2O2, (CCl3CO)2O / CH2Cl2 / 1.5 h / below 4 deg C View Scheme

1: 6.6 g / aq. CrO3, H2SO4 / acetone / 0.5 h / 5 °C 2: 2.7 g / CH2Cl2; diethyl ether / 0.17 h 3: 71.6 percent / aq. H2O2, (CCl3CO)2O / CH2Cl2 / 1.5 h / below 4 deg C View Scheme

1: 6.9 g / DIBAH / 1,2-dimethoxy-ethane; hexane / 2 h / 5 °C 2: 6.6 g / aq. CrO3, H2SO4 / acetone / 0.5 h / 5 °C 3: 2.7 g / CH2Cl2; diethyl ether / 0.17 h 4: 71.6 percent / aq. H2O2, (CCl3CO)2O / CH2Cl2 / 1.5 h / below 4 deg C View Scheme

1: 2.7 g / CH2Cl2; diethyl ether / 0.17 h 2: 71.6 percent / aq. H2O2, (CCl3CO)2O / CH2Cl2 / 1.5 h / below 4 deg C View Scheme

dipotassium hydrogenphosphate; dihydrogen peroxide; trichloroacetonitrile in dichloromethane; water T=8 - 10°C; 23 h;

1.1: acetic acid / N,N-dimethyl-formamide / 0.5 h / 45 °C 1.2: 4 h 2.1: potassium carbonate / 0 - 20 °C 3.1: triethylamine / dichloromethane / 0 °C 4.1: potassium formiate; formic acid / acetic anhydride / 100 °C 5.1: .alpha.,.alpha.,.alpha.-trichloroacetamide; dihydrogen peroxide; dipotassium hydrogenphosphate / dichloromethane / 10 - 20 °C View Scheme