Multi-step reaction with 10 steps
1: 1.) hexamethyldisilazane, amonium sulfate / 1.) reflux, 3 h, 2.) chloroform, reflux, 24 h
2: 88 percent / NH3 / methanol / 24 h / Ambient temperature
3: 1.) pyridine / 1.) 100-110 deg C, 2 h, 2.) a) 0 deg C, 72 h, b) RT, 5 h
4: aq. NaOH / ethanol / 1.25 h / Heating
5: aq. NaOH / ethanol / 1.25 h / Heating
6: 59 percent / (diethylamido)sulfur trifluoride / CH2Cl2 / 1.5 h / Ambient temperature
7: 87 percent / HCl / CHCl3 / 0.75 h / 0 °C
8: 79 percent / pyridine / 48 h / 4 °C
9: 93 percent / phosphoryl chloride, triethylamine / acetonitrile / 2 h / Ambient temperature
10: 1.) conc. aq. NH3, 2.) NH3, methanol / 1.) dioxane, RT, 7 h, 2.) RT, 18 h
With
pyridine; hydrogenchloride; methanol; ammonium sulfate; ammonium hydroxide; sodium hydroxide; (diethylamido)sulfur trifluoride; ammonia; triethylamine; 1,1,1,3,3,3-hexamethyl-disilazane; trichlorophosphate;
In
methanol; ethanol; dichloromethane; chloroform; acetonitrile;
DOI:10.1021/jm00170a015