Sulfuric Acid → HCID 20442912, compound

Temperature

20 °C

1,3-Dichloro-5-(trifluoromethoxy)-4-methylbenzene (8.0 g, 33 mmol) and 5.0 g (78 mmol) of chloromethyl methyl ether were added to 50 ml of H2SO4 (98%) with stirring at 20° C. The temperature rose slowly to 30° C. The mixture was stirred for 15 hours, then poured into 200 ml of ice water and extracted with 2×100 ml portions of hexane. The hexane extracts were combined, washed with 100 ml of water, dried (MgSO4), filtered, and concentrated. The residue was dissolved in 50 ml of hexane, filtered and concentrated. The resulting white solid was dried (25° C./0.001 mm) to give 9.0 g of 1,3-dichloro-2-chloromethyl-4-methyl-5-(trifluoromethoxy)benzene.

1. customrose slowly to 30° C
2. stirringThe mixture was stirred for 15 hours
3. extractionextracted with 2×100 ml portions of hexane
4. washwashed with 100 ml of water
5. dry with materialdried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated
8. dissolutionThe residue was dissolved in 50 ml of hexane
9. filtrationfiltered
10. concentrationconcentrated
11. customThe resulting white solid was dried (25° C./0.001 mm)

ORD record

ord-eea921154afa41ae8317038a86e9dd43

Source dataset

uspto-grants-1984_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04476056