I am going to use a 50 ml teflon lined autoclave for doing hydrothermal synthesis and I am deeply concerned about its safety. The pressure limit inside the autoclave is 3MPa and temperature limit is 230 deg C.
The solvents which have slightly higher boiling points must be preferbly used (DMF, DEF, DMSO, DMA etc even ethanol can be used) instead of low bioiling points solvents (Chloroform, acetone, acetates etc). But main thing which should be be focussed is ratio of organic solvent is to water, try a mixature instead of pure organic solvents. The Organic counterpart must be in smaller ratio or you can vary the two accordingly in optimization of reaction conditions.
Caution: The most important thing which must be kept in mind is never go more than 35 ml volume of reaction mixture otherwise mishappening can be happen.