Multi-step reaction with 9 steps
1.1: N-chloro-succinimide / acetonitrile / 70 °C / Reflux
2.1: trichlorophosphate / N,N-dimethyl-formamide / 20 - 120 °C
2.2: 0 °C / pH 7
3.1: sodium hydride / N,N-dimethyl-formamide; mineral oil / 20 °C
3.2: 20 °C
4.1: trifluoroacetic acid / dichloromethane / 20 °C / Reflux
5.1: 16 h / 110 °C
6.1: hydrogen / nickel / methanol / 21 h
6.2: 72 h / 65 °C
7.1: caesium carbonate / 1,4-dioxane / 33 h / 100 °C
8.1: methanol; sodium hydroxide / 0.5 h / 50 °C
8.2: pH 2 - 3
9.1: (benzotriazo-1-yloxy)tris(dimethylamino)phosphonium hexafluorophosphate; N-ethyl-N,N-diisopropylamine / N,N-dimethyl-formamide / 15 h / 20 °C
With
methanol; N-chloro-succinimide; hydrogen; sodium hydride; (benzotriazo-1-yloxy)tris(dimethylamino)phosphonium hexafluorophosphate; caesium carbonate; N-ethyl-N,N-diisopropylamine; trifluoroacetic acid; sodium hydroxide; trichlorophosphate;
nickel; N,N-dimethyl-formamide;
In
1,4-dioxane; methanol; dichloromethane; N,N-dimethyl-formamide; acetonitrile; mineral oil;