1: With disodium hydrogenphosphate in acetonitrile T=20°C; Methylation; 2: With disodium hydrogenphosphate Hydrolysis; 18 h;

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triethylamine; POCl3 in dichloromethane addn. of POCl3 to a soln. of amide in CH2Cl2, stirring at 0°C for30 min, addn. of a soln. of chromium complex and amine in CH2Cl2, stirr ing for 24 h at 20°C; flash column chromy. (SiO2, pentane, then pentane/CH2Cl2 3:1), recrystn.(CH2Cl2/Et2O, -20°C); elem. anal.;

1: triethylamine; POCl3 / dichloromethane 2: benzene View Scheme

1: With diisobutylaluminium hydride in tetrahydrofuran; hexane T=-78°C; 1.5 h; Inert atmosphere; 2: With ammonia; iodine in tetrahydrofuran; hexane; water T=0 - 20°C; Inert atmosphere;

ethyl trifluoromethanesulphonate; L-Selectridereg; 1) CH2Cl2, r.t., 24h, 2) THF, -78 deg C, 1.5h; Yield given. Multistep reaction;

1.1: (R)-BINOL; triphenylarsine oxide; Sm(O-iPr)3 / tert-butyl hydroperoxide / tetrahydrofuran; decane / 12 h / 20 °C 2.1: Me3SiN3; Ph3AsO; Sm(O-iPr)3 / tetrahydrofuran; decane / 1 h / 20 °C 2.2: aq. HCl / tetrahydrofuran; decane; methanol / 20 °C 3.1: 98 percent / triethylamine; DMAP / CH2Cl2 / 2 h / 20 °C 4.1: 96 percent / H2 / Pd/C / ethyl acetate / 135 h / 20 °C / 760 Torr 5.1: SOCl2 / CHCl3 / 2 h / 20 °C 6.1: 89 mg / aq. NaOH / ethanol / 15 h / 60 °C 7.1: methanol; diethyl ether / 0.5 h / 20 °C 8.1: 11.0 mg / aq. HCl / methanol / 2 h / Heating View Scheme

sodium hydroxide; water Reflux;

phosphorus oxychloride; triethylamine in dichloromethane under Ar atm. to N,N-dimethyl-3-phenylacrylamide in CH2Cl2 was added POCl3 and stirred at 0°C for 30 min, W complex and NEt3 in CH2Cl2 were added, 20°C, 16 h; react. mixt. was evapd. at 20°C, residue was dissolved in CH2Cl2 and chromed. on silica; diastereomers were not isolated;

Fe3O4Rh; hydrazine hydrate in ethanol T=80°C; 14 h; Inert atmosphere;