Methyl Methacrylate → HCID 58659609, compound

Participants

Reaction Conditions

Reaction Steps

In an oven dried 300 mL round-bottom flask equipped with a reflux condenser were added 2,6-Dimethyl-tetrahydro-oxazolo[2,3-b]oxazol-7a-yl-methanol (789 g, 0.45 mol), methyl methacrylate (180.0 g, 1.80 mol), Prostab® 5415 (3.00 g, Ciba Specialty Chemicals, Basel, Switzerland) and titanium (iv) n-butoxide (6.00 g, 0.024 mol). The reaction content was heated to 110° C. for ˜8 hours GC analyses indicated ˜44% conversion. The reflux condenser was replaced with an oven dried distillation head and the distillate boiling between 60-70° C. collected. The distillation head was replaced with a reflux condenser and the reaction content heated to 120° C. for ˜4 hours, at the end of which GC analyses indicated the conversion to be ˜75%. Again the reflux condenser was replaced with a distillation head and the distillated boiling between 60-70° C. collected for ˜8 hours, at the end of which GC analyses indicated the conversion to be ˜90%. The reaction content was cooled to room temperature and the unreacted methyl methacrylate removed under vacuum and then the remaining reaction content vaccuum fractionally distilled affording four fractions:

Provenance & Evidence