Hydrochloric Acid → HCID 12418397, compound

Temperature

0 °C

Anhydrous aluminum chloride (8.4 g; 0.063 mole) was added portionwise over a period of 2 hours to a stirred mixture of cyclohexene (108 g; 1.32 moles) and chloral (97 g; 0.653 mole), the temperature of which was maintained at 0° C. The reaction was allowed to proceed for a further 1 hour at 0° C. and then poured into a mixture of ice and concentrated hydrochloric acid. The reaction mixture was extracted three times with ether and the combined extracts washed with water (2×200 ml). The dried (MgSO4) extract was evaporated and the residue distilled to give crude product (116 g; 85% purity as judged by G.L.C.), b.p. 90°-94° C./0.1 mm. The crude product was redistilled through a Widmer column to give 1-(2-cyclohexen-1-yl)-2,2,2-trichloroethanol (98 g; 65% yield based on chloral; 93% purity as judged by G.L.C.) b.p. 67°-68° C./0.03 mm. A sample was redistilled for analysis.

1. extractionThe reaction mixture was extracted three times with ether
2. washthe combined extracts washed with water (2×200 ml)
3. dry with materialThe dried (MgSO4)
4. extractionextract
5. customwas evaporated
6. distillationthe residue distilled
7. customto give crude product (116 g; 85% purity as judged by G.L.C.), b.p. 90°-94° C./0.1 mm
8. distillationThe crude product was redistilled through a Widmer column

ORD record

ord-810fbbe7af7b46b4b4fbf35f135ef7ad

Source dataset

uspto-grants-1981_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04249015