triethylamine in acetonitrile T=20°C; 12 h;

sodium carbonate in acetonitrile T=130°C; 2 h;

1.1: 1-chloroethyl chlorocarbonate / 1,2-dichloro-ethane / 6 h / Reflux 1.2: 4 h / Reflux 2.1: triethylamine / acetonitrile / 12 h / 20 °C View Scheme

1.1: hydrogenchloride 2.1: diethyl ether / -45 °C 2.2: -78 °C 3.1: 2 h / 120 °C 4.1: acetic acid; zinc / 16 h / 20 °C 5.1: triethylamine / acetonitrile / 5 h / 80 °C / |Inert atmosphere 6.1: dichloromethane / 20 h / 45 °C / |Inert atmosphere; |Cooling with ice 7.1: 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane; potassium fluoride / acetonitrile / 0.17 h / 80 °C / |Sealed tube View Scheme

1: acetic acid; zinc / 16 h / 20 °C 2: triethylamine / acetonitrile / 5 h / 80 °C / |Inert atmosphere 3: dichloromethane / 20 h / 45 °C / |Inert atmosphere; |Cooling with ice 4: 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane; potassium fluoride / acetonitrile / 0.17 h / 80 °C / |Sealed tube View Scheme

1.1: hydrogenchloride; water / |Heating 2.1: trichlorophosphate 3.1: hydrogenchloride 4.1: diethyl ether / -45 °C 4.2: -78 °C 5.1: 2 h / 120 °C 6.1: acetic acid; zinc / 16 h / 20 °C 7.1: triethylamine / acetonitrile / 5 h / 80 °C / |Inert atmosphere 8.1: pyridine / dichloromethane / 1.5 h / 20 °C / |Inert atmosphere; |Cooling with ice 9.1: hydrogenchloride / methanol / 80 °C 10.1: 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane; potassium fluoride / acetonitrile / 0.08 h / 110 °C / |Sealed tube View Scheme

1.1: trichlorophosphate 2.1: hydrogenchloride 3.1: diethyl ether / -45 °C 3.2: -78 °C 4.1: 2 h / 120 °C 5.1: acetic acid; zinc / 16 h / 20 °C 6.1: triethylamine / acetonitrile / 5 h / 80 °C / |Inert atmosphere 7.1: dichloromethane / 20 h / 45 °C / |Inert atmosphere; |Cooling with ice 8.1: 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane; potassium fluoride / acetonitrile / 0.17 h / 80 °C / |Sealed tube View Scheme

1: 2 h / 120 °C 2: acetic acid; zinc / 16 h / 20 °C 3: triethylamine / acetonitrile / 5 h / 80 °C / |Inert atmosphere 4: dichloromethane / 20 h / 45 °C / |Inert atmosphere; |Cooling with ice 5: 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane; potassium fluoride / acetonitrile / 0.17 h / 80 °C / |Sealed tube View Scheme

1: triethylamine / acetonitrile / 5 h / 80 °C / |Inert atmosphere 2: dichloromethane / 20 h / 45 °C / |Inert atmosphere; |Cooling with ice 3: 4,7,13,16,21,24-hexaoxa-1,10-diazabicyclo[8.8.8]hexacosane; potassium fluoride / acetonitrile / 0.17 h / 80 °C / |Sealed tube View Scheme

1.1: hydrogenchloride 2.1: diethyl ether / -45 °C 2.2: -78 °C 3.1: 2 h / 120 °C 4.1: acetic acid; zinc / 16 h / 20 °C 5.1: sodium carbonate / acetonitrile / 2 h / 130 °C View Scheme