反应条件
1: 1.) cc. H2SO4, 2.) NaH / 1.) 4 deg C, 16 h, 2.) DMF, 40 deg C 2: 125.9 g / SnCl4 / CH2Cl2 / 35 h / 3 °C 3: pyridine, 4-(dimethylamino)-pyridine / 17 h 4: 1.) N,O-bis(trimethylsilyl)acetamide, 2.) TfOSiMe3 / 1.) ClCH2CH2Cl, reflux, 10 min, 2.) ClCH2CH2Cl, 70 deg C, 20 h 5: 1,8-diazabicyclo<5.4.0>undec-7-ene / acetonitrile / 10 h 6: 98 percent / 30percent NaOMe / methanol / 3 h / Ambient temperature 7: 98 percent / NaH / tetrahydrofuran / 40 - 70 °C 8: H2 / 5percent Pd/C / tetrahydrofuran / Ambient temperature 9: 30percent NaOMe / methanol / Ambient temperature; pH 11 10: 84 percent / H2, NaOAc / 5percent Pd/C / methanol / 45 °C / 2250.2 Torr View Scheme
参考文献
Martin
Helvetica Chimica Acta, 1995 , vol. 78, # 2 p. 486 - 504
