Acetic Acid → HCID 23195142, compound

Participants

Reaction Steps

A mixture of 260B (1.30 g, 5.75 mmol), thiourea (524 mg, 6.90 mmol), acetic acid (2 ml) and EtOH (10 ml) was refluxed overnight. The reaction mixture was cooled to room temperature and the solid that separated out was filtered. The filtrate was concentrated and made acidic using 1N HCl. The aqueous solution was washed with EtOAc (2×25 mL), cooled to 0° C. and basified with 2N NaOH. The sodium hydroxide layer was re-extracted with EtOAc (2×25 mL), washed with water (25 mL), dried over Na2SO4 and concentrated under reduced pressure to give 260C (390 mg, 45%) 1NMR (CDCl3) δ 8.45 (d, 2H), 7.06 (d, 2H), 2.58 (s, 2H), 1.06 (s, 6H)

Provenance & Evidence