hydrogenchloride in acetone

1: 8 percent / ZnCl2 / ethyl acetate / 12 h / 0 °C 2: 1) BuLi, HMPT / 1) THF, hexane, -78 deg C, 30 min.; 2) THF, a) -78 deg C, 1 h, b) 0 deg C, 14 h, c) room temperature, 1 h 3: 95 percent / chromatography, hydrolysis 4: 77 percent / MeONa / methanol / 12 h 5: 90 percent / MeONa / methanol; tetrahydrofuran / 240 h / Ambient temperature View Scheme

Na2Si3O7; magnesium hydrogen phosphate; nitrogen T=350°C; P=40 Torr;

Na2Si3O7; magnesium hydrogen phosphate; nitrogen T=350°C; P=40 Torr;

in diethyl ether

1: potassium hydroxide / 140 °C 2: nitrogen; magnesium hydrogenphosphate sodium silicate / 350 °C / 40 Torr View Scheme

1: 1.) tert-butyllithium / 1.) THF, pentane, -78 deg C to -20 deg C, 30 min; -20 deg C, 30 min, 2.) -78 deg C 2: 90 percent Spectr. / 0.20 M aq. HCl / acetone / 2 h View Scheme

(i), (ii) aq. KOH, O2, THF; Multistep reaction;

1: 1.) tert-butyllithium / 1.) THF, pentane, -78 deg C to -20 deg C, 30 min; -20 deg C, 30 min, 2.) -78 deg C 2: 10 percent Spectr. / 0.20 M aq. HCl / acetone / 2 h View Scheme