反应条件
1: 92 percent / aq. sodium bicarbonate / ethyl acetate / 1 h / 0 °C 2: 4.36 g / diisobutylaluminium hydride (Dibal) / toluene / 1.85 h / -78 °C 3: 1. diisopropylamine, n-butyllithium / 1. THF, -78 deg C, 0.25h, 2. THF, -78 deg C, 0.25h 4: 0.71 g / p-toluenesulphonic acid monohydrate / methanol / 0.5 h 5: 72 percent / K2CO3 / methanol; H2O / 2 h 6: 1. triflic anhydride, pyridine, 2. sodium iodide / 1. CH2Cl2, 0 deg C, 1h, 2. ethylene glycol dimethyl ether (DME), a.) 0 deg C to r.t., b.) 1.2h 8: methanol; diethyl ether 9: pyridinium dichromate (PDC) / dimethylformamide / 40 °C 10: diethyl ether; dimethylformamide 11: 91 mg / 2.5percent aq. potassium hydroxide / methanol / 3.5 h / Heating 12: 67 percent / trifluoroacetic acid (TFA) / CH2Cl2 / a.) 0 deg C, 0.5h, b.) r.t., 0.25h View Scheme
参考文献
Baldwin, Jack E.; Moloney, Mark G.; Parsons, Andrew F.
Tetrahedron, 1990 , vol. 46, # 20 p. 7263 - 7282