Hydrochloric Acid → HCID 10125073, compound

Prepared according to Zaidlewicz, M.; et al; Tetrahedron:Asymmetry; 2003, 14, 1659-1664: Magnesium chloride (11.4 g, 120 mmol) was added at room temperature to a solution of 2-ethylphenol (9.77 g, 80 mmol) in acetonitrile (100 mL), followed by triethylamine (42 mL, 300 mmol). Paraformaldehyde (16.2 g, 540 mmol) was then added portionwise to the stirred suspension and the mixture was heated at reflux for 3 hours. The mixture was cooled to room temperature then poured into a vigorously stirred mixture of 250 mL of 5% HCl and 150 mL of diethyl ether. The organic phase was separated, and the aqueous layer re-extracted with 100 mL of ether. The combined organic extracts were washed with brine, dried over sodium sulphate and the solvent removed under reduced pressure to give 11.5 g of 9 as a yellow oil which was used without further purification:

1. customPrepared
2. temperaturethe mixture was heated
3. temperatureat reflux for 3 hours
4. customThe organic phase was separated
5. extractionthe aqueous layer re-extracted with 100 mL of ether
6. washThe combined organic extracts were washed with brine
7. dry with materialdried over sodium sulphate
8. customthe solvent removed under reduced pressure

ORD record

ord-7021500de3824ce1a3148b03e3b463ae

Source dataset

uspto-grants-2012_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08198302B2