Sample heating with a laser beam facilitates time-dependent magic angle spinning (MAS) NMR spectroscopy of high-temperature reactions in situ. The methanol-to-gasoline conversion (MTG process) was monitored by C-13 MAS NMR spectroscopy using the stop-and-go method in addition to the continuous heating of sealed samples. It was found that effective alkane formation is forced by interrupted laser heating. With a decrease of the dimethyl ether concentration a constant concentration of methanol was observed under both continuous and interrupted heating conditions. Copyright (C) 1999 John Wiley & Sons, Ltd.