trichlorophosphate in acetonitrile T=20°C; 7 h; Reflux;

trichlorophosphate

1: acetic acid; bromine 2: phosphoryl chloride View Scheme

1: diphenyl ether; biphenyl / 180 °C 2: phosphoryl chloride View Scheme

1: aqueous NaOH 2: diphenyl ether; biphenyl / 180 °C 3: phosphoryl chloride View Scheme

1: bromine; iodine; acetic acid / 2 h / Inert atmosphere 2: trichlorophosphate / 1 h / Inert atmosphere; Reflux View Scheme

1.1: 0.5 h / |Reflux 1.2: 0.67 h / |Reflux 2.1: diphenylether / 0.5 h / 250 °C / |Inert atmosphere 3.1: acetic acid / 0.17 h / |Reflux 3.2: 2 h / |Reflux 4.1: trichlorophosphate / acetonitrile / 7 h / 20 °C / |Reflux View Scheme

1.1: diphenylether / 0.5 h / 250 °C / |Inert atmosphere 2.1: acetic acid / 0.17 h / |Reflux 2.2: 2 h / |Reflux 3.1: trichlorophosphate / acetonitrile / 7 h / 20 °C / |Reflux View Scheme

1.1: hydrogenchloride / dichloromethane; diethyl ether / 1 h / 5 - 20 °C 1.2: 5 h / |Reflux 2.1: palladium diacetate; 9,9-dimethyl-4,5-bis(diphenyl-phosphino)xanthene; caesium carbonate / toluene / 1.5 h / 120 °C / |Inert atmosphere; |Microwave irradiation 3.1: bis-triphenylphosphine-palladium(II) chloride; sodium acetate / N,N-dimethyl acetamide / 1 h / 150 °C / |Inert atmosphere; |Microwave irradiation View Scheme