Hydrochloric Acid → HCID 19813279, compound

Participants

Reaction Steps

Isopropyl 2-(1,3-dithiol-2-ylidene)-2-(ethoxycarbonyloxy-carbonyl)acetate (13.2 g) and proline (4.6 g) was dissolved in DMF (60 ml). The mixture was stirred at room temperature for 24 hrs, thereto was added conc-HCl (20 ml) and stirred for a further 2 hrs. The reaction mixture was poured into ice water and basified to pH=12 with aqueous sodium hydroxide solution. The mixture was washed with methylene chloride and the aqueous layer was acidified to pH=2 with dil-HCl. The solid formed was filtered and recrystallized from ethyl acetate and n-hexane to obtain the pure product (12.5 g, 91%).

Provenance & Evidence