Hydrochloric Acid → HCID 68726754, compound

Participants

Reaction Steps

At 5° C., a solution of the previously obtained 7-methylenespiro[4.5]decane-6-carboxylic acid (1.2 g, 6.2 mmol) in DMF (30 ml) was treated with K2CO3 (0.94 g, 6.8 mmol). The resulting mixture was stirred for 30 min., treated with ethyl iodide (0.75 ml, 9.3 mmol), stirred at 20° C. for 2 h, poured into cold 2N aqueous HCl (20 ml), and extracted twice with hexane (50 ml). The combined organic phases were washed with water (50 ml), with a saturated aqueous solution of NaCl (50 ml), dried (MgSO4), and concentrated. FC (90 g SiO2, hexane/MTBE 98:2) of the crude product (1.23 g) gave ethyl 7-methylenespiro[4.5]decane-6-carboxylate (0.69 g, 50%). Boiling point: 90° C. (0.08 mbar).

Provenance & Evidence