Methanol → HCID 9855500, compound

The distilled acid, 20 g, containing 14% of unreacted heptanoic acid, was treated at room temperature (22° C.) with 100 g absolute methanol and 0.4 ml of the methanol complex solution of boron trifluoride. After standing for 1 hr., 100 ml of water was added and the layers were separated. The water was extracted twice with 100 ml portions of hexane. The combined layer was freed from hexane by evaporation, and the residue was fractionally distilled. The forerun 2.7 g, boiling range 77°-120° C. vapor temperature at 20mm Hg contained mostly the methyl ester of the saturated acid. The residue, 15.4 g contained 98% acid by titration and consisted of 99% α-pentylacrylic acid according to the gas chromatographic analysis.

1. customthe layers were separated
2. extractionThe water was extracted twice with 100 ml portions of hexane
3. customThe combined layer was freed from hexane by evaporation
4. distillationthe residue was fractionally distilled

ORD record

ord-d301b251789d4221916c03d7ca0ba3d5

Source dataset

uspto-grants-1984_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04477384