80841-78-7,is a common compound. C5H5ClO3.In an article, once mentioned the new application about 80841-78-7.
To BIC (110 g, 1 eq) was added acetone (385 mL, 3.5 vol) at 25C – 30C, and the mixture was dissolved by stirring for 5 min. Sodium carbonate (20.85 g, 1.3 eq) and potassium iodide (0.25 g, 0.01) were added, and the mixture was stirred for 10 min. A solution of 4-chloromethyl-5-methyl-2-oxo-1,3-dioxolene (31.456 g, 1.4 eq) in acetone (165 mL, 1.5 vol) was added thereto. The reaction mixture was heated to 45C – 50C, and stirred at the same temperature for 12 hr. Using TLC (thin layer chromatography) (TLC eluent: 10% methanol/methylene chloride, detection method: UV), complete disappearance of BIC was confirmed. The reaction mixture was cooled to 25C – 30C. Then, the solvent contained in the reaction mixture was evaporated under reduced pressure at 40C – 45C. To the obtained residue were added 10% brine (550 mL, 5 vol) and toluene (550 mL, 5 vol). Furthermore, the mixture was adjusted to pH 7 – 8 by adding 5% hydrochloric acid (33 mL), stirred for 10 min, left standing for 5 min and partitioned. The aqueous layer was extracted with toluene (2×330 mL, 2×3 vol). The extracts were combined with the organic layer, 10% brine (550 mL, 5 vol) was added, and the mixture was stirred for 5 min, left standing for 45 min, partitioned, and concentrated under reduced pressure at 40C – 45C to give TOLM (110 g, 90%). [0306] To the obtained TOLM was added acetone (110 mL, 1 vol), and the mixture was stirred at 25C – 30C for 30 min. n-Heptane (440 mL, 4 vol) was added, and the mixture was cooled to 5C – 10C and stirred at 5C – 10C for 30 min, whereby precipitation of a solid was confirmed. The solid (80 g, 66%) was collected by filtration, and blast dried. To the obtained solid was added isopropyl alcohol (400 mL, 5 vol), and the mixture was heated to 50C – 55C and stirred at 50C – 55C for 1 hr. Then, the mixture was cooled to 25C – 30C, and stirred at 25C – 30C for 1 hr. The resulting solid was filtered and suction-filtered for 10 min to give TOLM (76 g, 62%).
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Reference£º
Patent; API Corporation; SEKI, Masahiko; EP2891650; (2015); A1;,
1,3-Benzodioxole – Wikipedia
Dioxole | C3H4O2 – PubChem