Potassium ethanethioate → HCID 54193495, compound

2.11 g (10.8 mmol) of (2R,3S)-2-bromo-3-methylpentanoic acid obtained in the Synthesis Example C-1 was dissolved in 43 ml of acetonitrile and 1.42 g of potassium thioacetate was added thereto at 0° C. The mixture was stirred at0° C. for 30 minutes and then at room temperature for 5 hours. After filtering off the insoluble matters, the filtrate was concentrated. To the residue were added ether and a saturated aqueous solution of sodium hydrogencarbonate, followed by separation. The aqueous phase was acidified by adding a 2N aqueous solution of hydrochloric acid at a low temperature and then extracted with ether. The ether phase was washed with a saturated aqueous sodium chloride, dried over anhydrous magnesium sulfate and concentrated. Thus, 1.68 g of the title compound was obtained as a colorless oil (yield 82%).

1. customat 0° C
2. waitat room temperature for 5 hours
3. filtrationAfter filtering off the insoluble matters
4. concentrationthe filtrate was concentrated
5. additionTo the residue were added ether
6. customa saturated aqueous solution of sodium hydrogencarbonate, followed by separation
7. additionby adding a 2N aqueous solution of hydrochloric acid at a low temperature
8. extractionextracted with ether
9. washThe ether phase was washed with a saturated aqueous sodium chloride
10. dry with materialdried over anhydrous magnesium sulfate
11. concentrationconcentrated

ORD record

ord-e7a02601b1f74175b70264d97976d204

Source dataset

uspto-grants-1997_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05679671