Real time HR-MAS NMR: application in reaction optimization, mechanism elucidation and kinetic analysis for heterogeneous reagent catalyzed small molecule chemistry.
A novel application of in situ (1)H high-resolution magic angle spinning (HR-MAS) NMR technique for real-time monitoring of H(2)SO(4)-silica promoted formation of 2, 2-disubstituted quinozolin-4(3H)-ones is reported. The detailed NMR spectroscopic data led to elucidation of the mechanism, reaction optimization, kinetics and quantitative analysis of the product accurately and efficiently. The translation of the optimized parameters obtained by (1)H HR-MAS NMR in the wet laboratory provided similar results. It is proposed that (1)H HR-MAS has a potential utility for optimization of various organic transformations in solid supported catalyzed reactions.
Sopisticated Analytical Instrument Facility, Central Drug Research Institute, Chattar Manzil Palace, Lucknow, India 226 001, India.
Abhijeet Deb
AD
Roy
K
K
Jayalakshmi
Somnath
S
Dasgupta
Raja
R
Roy
Balaram
B
Mukhopadhyay
D002384:Catalysis; D007700:Kinetics; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D009930:Organic Chemicals / Q000737:chemistry; D052999:Quinazolinones / Q000737:chemistry*; D012822:Silicon Dioxide
D009930:Organic Chemicals; D052999:Quinazolinones; D012822:Silicon Dioxide