Hydrochloric Acid → HCID 14149942, compound

A 500 ml round-bottom flask was initially charged with 51.1 g of hydroxyethyl acrylate in 100 ml of pyridine/toluene (1:1, v/v) together with 0.05 g of 2,6-di-tert-butyl-4-methylphenol at 0° C. and 65.0 g of benzoyl chloride were slowly added dropwise. The mixture was stirred at room temperature until the hydroxyethyl acrylate content had fallen below 0.1%. Thereafter, the mixture was poured onto 0.5 l of ice-water and acidified with 1 N aqueous hydrochloric acid. The aqueous phase was extracted three times with 0.5 l each time of tert-butyl methyl ether. The organic phase was washed with 10% sodium hydrogencarbonate solution, dried over sodium sulfate and filtered. Another 0.05 g of 2,6-di-tert-butyl-4-methylphenol was added and the organic solvents were distilled off. The product was obtained as a colorless oil.

1. extractionThe aqueous phase was extracted three times with 0.5 l each time of tert-butyl methyl ether
2. washThe organic phase was washed with 10% sodium hydrogencarbonate solution
3. dry with materialdried over sodium sulfate
4. filtrationfiltered
5. additionAnother 0.05 g of 2,6-di-tert-butyl-4-methylphenol was added
6. distillationthe organic solvents were distilled off
7. customThe product was obtained as a colorless oil

ORD record

ord-0e4cc40b72ff42edb3332eff00333169

Source dataset

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09057950B2