Multi-step reaction with 5 steps
1: 1.) NaH / 1.) DMF, RT, 15 min, 2.) DMF, RT, 2 h
2: 88 percent / NaClO2, NaH2PO4, 2-methyl-2-butene / N,N-dimethyl-acetamide; H2O / 2 h / Ambient temperature
3: 1.) diphenylphosphoryl azide, Et3N / 1.) toluene, reflux, 2 h, 2.) toluene, reflux, 8 h
4: 1.) NaH / 1.) DMF, RT, 15 min, 2.) DMF, 60 deg C, 3 h
5: 81 percent / H2 / 10 percent Pd/C / methanol; ethyl acetate / 12 h / Ambient temperature
With
sodium chlorite; sodium dihydrogenphosphate; 2-methyl-but-2-ene; diphenylphosphoranyl azide; hydrogen; sodium hydride; triethylamine;
palladium on activated charcoal;
In
methanol; N,N-dimethyl acetamide; water; ethyl acetate;
DOI:10.1248/cpb.47.226
