Dimethyl Ether → HCID 11356486, compound

Participants

Reaction Steps

To a stirred mixture of 116.0 g methyl-trans-3-methoxyacrylate and 530.0 g trimethyl ortho formate were added 5.0 g FeCl3. The mixture was heated to 35° C. for 30 hours with an additional 1.0 g FeCl3 being added every 6 hours. The mixture was cooled to room temperature and neutralized by addition of 30% sodium methylate solution. After stirring for 2 hours, 30.0 g PEG-dimethylether (mg=1000) were added. The trimethyl ortho formate excess was recovered by fractional distillation. Flash-distillation of the remaining material gave 155.4 g colorless liquid (80% of theoretical based on converted methyl-trans-3-methoxyacrylate) of boiling point 100° C./4 mm Hg. A GC-analysis of the liquid revealed an assay of >99% (FID-detection).

Provenance & Evidence