Multi-step reaction with 4 steps
1.1: oxalyl dichloride; N,N-dimethyl-formamide / dichloromethane / 4 h / 20 °C
2.1: 2,2,6,6-tetramethylpiperidinylmagnesium chloride lithium chloride complex / tetrahydrofuran / 0.5 h / 20 °C
2.2: 0.5 h / -30 °C
2.3: 5 h / -30 - 10 °C
3.1: pyridine hydrogenfluoride / tetrahydrofuran / 48 h / 20 - 40 °C
4.1: (1R,7R)-9,9-dimethyl-4-(N-phenyl-2-pyridylamino)-2,2,6,6-tetraphenyl-3,5,8,10-tetraoxa-4-phosphabicyclo[5.3.0]decane; tris-(dibenzylideneacetone)dipalladium(0) / acetonitrile / 6 h / 20 °C / Molecular sieve; Inert atmosphere
With
tris-(dibenzylideneacetone)dipalladium(0); 2,2,6,6-tetramethylpiperidinylmagnesium chloride lithium chloride complex; oxalyl dichloride; (1R,7R)-9,9-dimethyl-4-(N-phenyl-2-pyridylamino)-2,2,6,6-tetraphenyl-3,5,8,10-tetraoxa-4-phosphabicyclo[5.3.0]decane; pyridine hydrogenfluoride; N,N-dimethyl-formamide;
In
tetrahydrofuran; dichloromethane; acetonitrile;
4.1: |Nazarov Cyclization;
DOI:10.1002/anie.201500881