Multi-step reaction with 6 steps
1: 41 percent / N,N-Dimethylanilin / xylene / 2 h / 180 °C
2: 1) NaH / 1) DMF, 0 deg C, 1 h 2) 0 deg C, 1 h 3) r.t., 3 h
3: 1) Lithiumdiisopropylamid / 1) THF, -78 deg C, 30 min 2) THF, -78 deg C, 10 h 3) r.t., 10 h
4: 91 percent / NH2OH*HCl, NaOH / ethanol; H2O / 12 h / Heating
5: 45 percent / Zn, 25percent NH3 / ethanol / 5 h / Heating
6: 57 percent / BBr3 / CH2Cl2 / 1) -78 deg C, 3 h 2) r.t., 20 h 3) reflux, 2 h
With
ammonium hydroxide; sodium hydroxide; hydroxylamine hydrochloride; boron tribromide; sodium hydride; N,N-dimethyl-aniline; zinc; lithium diisopropyl amide;
In
ethanol; dichloromethane; water; xylene;
DOI:10.1002/ardp.2503241003