Hydrochloric Acid → HCID 20285690, compound

A mixture of 61.59 g. (0.368 mol) of 2,5-dichloro-3-methylthiophene, 13.1 g. of paraformaldehyde and 3.1 g. of zinc chloride was heated to 55° C. Hydrogen chloride gas was passed through the mixture for 7.25 hours. The resulting mixture was cooled and poured into a mixture of ether and ice water. The organic phase was separated and washed with sodium chloride solution, sodium bicarbonate solution and sodium chloride solution again. Evaporation of the dried solvent gave a dark brown oil which was distilled under reduced pressure to yield 3-chloromethyl-2,5-dichloro-4-methylthiophene as a pale yellow liquid, b.p. 87°-92° C./0.75 mm.

1. additionA mixture of 61.59 g
2. temperatureThe resulting mixture was cooled
3. customThe organic phase was separated
4. washwashed with sodium chloride solution, sodium bicarbonate solution and sodium chloride solution again
5. customEvaporation of the dried solvent
6. customgave a dark brown oil which
7. distillationwas distilled under reduced pressure

ORD record

ord-62907893e46a44dd9990e189157a856b

Source dataset

uspto-grants-1978_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04116975