trichlorophosphate in N-methyl-acetamide; water

trichlorophosphate in water

boron tribromide in dichloromethane T=-30 - 25°C;

1: 78 percent / hydrazine hydrate / 2 h / Heating 2: 63 percent / sodium nitrite, hydrochloric acid (2M), acetic acid (glacial) / H2O / 1 h / -10 °C 3: 93 percent / toluene / 2.5 h / Heating 4: 8.7 g / sodium hydroxide (20percent) / 60 °C 8: 28.8 g / fluoroboric acid, sodium nitrite / H2O 9: 7.6 g / warming, distillation 10: 1.456 g / boron tribromide / CH2Cl2 / 52 h View Scheme

1: 84 percent / sodium hydroxide / heating 5: 28.8 g / fluoroboric acid, sodium nitrite / H2O 6: 7.6 g / warming, distillation 7: 1.456 g / boron tribromide / CH2Cl2 / 52 h View Scheme

2: 28.8 g / fluoroboric acid, sodium nitrite / H2O 3: 7.6 g / warming, distillation 4: 1.456 g / boron tribromide / CH2Cl2 / 52 h View Scheme

1: 93 percent / toluene / 2.5 h / Heating 2: 8.7 g / sodium hydroxide (20percent) / 60 °C 6: 28.8 g / fluoroboric acid, sodium nitrite / H2O 7: 7.6 g / warming, distillation 8: 1.456 g / boron tribromide / CH2Cl2 / 52 h View Scheme

1: 63 percent / sodium nitrite, hydrochloric acid (2M), acetic acid (glacial) / H2O / 1 h / -10 °C 2: 93 percent / toluene / 2.5 h / Heating 3: 8.7 g / sodium hydroxide (20percent) / 60 °C 7: 28.8 g / fluoroboric acid, sodium nitrite / H2O 8: 7.6 g / warming, distillation 9: 1.456 g / boron tribromide / CH2Cl2 / 52 h View Scheme

1: 7.6 g / warming, distillation 2: 1.456 g / boron tribromide / CH2Cl2 / 52 h View Scheme

4: 28.8 g / fluoroboric acid, sodium nitrite / H2O 5: 7.6 g / warming, distillation 6: 1.456 g / boron tribromide / CH2Cl2 / 52 h View Scheme