disodium hydrogenphosphate; sodium amalgam in methanol T=0°C; 1 h; Yield given;

1: 99.2 percent / H2O2 / acetic acid / 2 h / 100 °C 2: n-butyllithium / 1.) hexane, ethyl ether, -70 deg C, 25 min, 2.) from - 70 deg C up to room temperature in 20 min 3: diethyl ether / 1.) -10 deg C, 2.) reflux 25 min 4: sodium amalgam, disodium hydrogen phosphate / methanol / 1 h / 0 °C View Scheme

1: n-butyllithium / 1.) hexane, ethyl ether, -70 deg C, 25 min, 2.) from - 70 deg C up to room temperature in 20 min 2: diethyl ether / 1.) -10 deg C, 2.) reflux 25 min 3: sodium amalgam, disodium hydrogen phosphate / methanol / 1 h / 0 °C View Scheme

1: 99.2 percent / azoisobutyrinitrile / 90 °C 2: 99.2 percent / H2O2 / acetic acid / 2 h / 100 °C 3: n-butyllithium / 1.) hexane, ethyl ether, -70 deg C, 25 min, 2.) from - 70 deg C up to room temperature in 20 min 4: diethyl ether / 1.) -10 deg C, 2.) reflux 25 min 5: sodium amalgam, disodium hydrogen phosphate / methanol / 1 h / 0 °C View Scheme