Sulfuric Acid → HCID 13592062, compound

Temperature

50 °C

0.9 g of 2 allyl-5-methoxymethoxy-4,6,7-trimethyl-1,3-benzoxathiole (prepared as described in Example 89) was dissolved in 8 ml of acetic acid, and 3 drops of 10% v/v aqueous sulfuric acid were added to the resulting solution, which was then heated at 50° C. for 30 minutes. The solution was then cooled down to room temperature, and the reaction mixture was condensed by evaporation under reduced pressure. The condensate was dissolved in benzene, and the solution was washed with water and then dried over anhydrous sodium sulfate. The benzene was distilled off, and the resulting crude product was purified by silica gel Lobar column chromatography. The title compound, melting at 78.5°-79.5° C., was obtained from the fraction eluted with benzene.

1. temperatureThe solution was then cooled down to room temperature
2. customcondensed
3. customby evaporation under reduced pressure
4. dissolutionThe condensate was dissolved in benzene
5. washthe solution was washed with water
6. dry with materialdried over anhydrous sodium sulfate
7. distillationThe benzene was distilled off
8. customthe resulting crude product was purified by silica gel Lobar column chromatography

ORD record

ord-111c3b0de1184a2babf10d2133193ee3

Source dataset

uspto-grants-1987_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04691027