反应详情

温度

0 °C

A solution of tert-butyl-3-tert-butoxy-2-ethyloxycarbonyl-5-thiophenecarboxylate (11.5 g, 35 mmol) in dioxane with NaOH (2N) (34.5 ml, 70 mmol) was heated for 1.45 hours at 50° C. The mixture was cooled to 0° C., neutralized with HCl (2N), and the solvent evaporated. The residue was triturated with a concentrated aqueous solution of Na2CO3 (400 ml) and ether (200 ml). The aqueous phase was recovered, cooled to 0° C., acidified with HCl (5N) and extracted with ether. After drying, concentration of the etheral phase, and purification by flash silica gel chromatography, the title compound was obtained (3.45 g).

1. customthe solvent evaporated
2. customThe residue was triturated with a concentrated aqueous solution of Na2CO3 (400 ml) and ether (200 ml)
3. customThe aqueous phase was recovered
4. temperaturecooled to 0° C.
5. extractionextracted with ether
6. customAfter drying
7. customconcentration of the etheral phase, and purification by flash silica gel chromatography