Hydrochloric Acid → HCID 86717689, compound

In a 300-mL recovery flask were put 3.1 g (11 mmol) of 1-(3-chloro-2-fluorophenyl)-2-naphthol, 70 mL of N-methyl-2-pyrrolidone, and 4.2 g (31 mmol) of potassium carbonate, and this mixture was stirred at 150° C. in air for 7 hours. After stirring, about 50 mL of water and about 50 mL of hydrochloric acid (1.0 mol/L) were added to the resulting mixture. To the resulting solution was added about 100 mL of ethyl acetate; then, the aqueous layer was subjected to extraction with ethyl acetate three times. The solution of the extract combined with the organic layer was washed with a saturated aqueous solution of sodium hydrogen carbonate and a saturated aqueous solution of sodium chloride, and magnesium sulfate was then added. The mixture was gravity-filtered, and the resulting filtrate was concentrated to give 2.9 g of a pale brown solid of a target substance in a yield of over 99%.

1. customIn a 300-mL recovery flask were put
2. extractionthen, the aqueous layer was subjected to extraction with ethyl acetate three times
3. washwas washed with a saturated aqueous solution of sodium hydrogen carbonate
4. additiona saturated aqueous solution of sodium chloride, and magnesium sulfate was then added
5. filtrationThe mixture was gravity-filtered
6. concentrationthe resulting filtrate was concentrated

ORD record

ord-7e8ee61644f0473a9a1cc9703a9b450d

Source dataset

uspto-grants-2016_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09368732B2