Multi-step reaction with 5 steps
1.1: N-chloro-succinimide / N,N-dimethyl-formamide / 6 h / 20 °C / Inert atmosphere
2.1: 2,2,6,6-tetramethylpiperidinyl magnesium chloride-lithium chloride / tetrahydrofuran / 25 °C / Inert atmosphere
2.2: 0.25 h / 25 °C / Inert atmosphere
2.3: 4 h / 25 °C / Inert atmosphere
3.1: 2,2,6,6-tetramethylpiperidinyl magnesium chloride-lithium chloride / tetrahydrofuran / 25 °C / Inert atmosphere
3.2: 0.25 h / Inert atmosphere
3.3: 3 h / -20 - 20 °C / Inert atmosphere
4.1: palladium 10% on activated carbon; ammonium formate / ethanol; water / 5 h / 120 °C / Inert atmosphere; Microwave irradiation
5.1: 2,2,6,6-tetramethylpiperidinyl magnesium chloride-lithium chloride / tetrahydrofuran / -50 °C / Inert atmosphere
5.2: 1 h / -50 - 20 °C / Inert atmosphere
With
N-chloro-succinimide; palladium 10% on activated carbon; 2,2,6,6-tetramethylpiperidinyl magnesium chloride-lithium chloride; ammonium formate;
In
tetrahydrofuran; ethanol; water; N,N-dimethyl-formamide;
DOI:10.1002/chem.201002506