反应详情

A solution of product from Example 39B (0.35 g, 0.75 mmol) in methylene chloride (10 ml) was treated with vinyl chloroformate (0.1 mL, 1.2 mmol), stirred at ambient temperature for 16 hours, concentrated to dryness, treated with ethanol (10 mL), treated with 6N HCl (3 mL), refluxed for 5 hours and concentrated to dryness, Purification of the residue on silica gel (10:90:1 ethanol/methylene chloride/saturated ammonium hydroxide) provided the title compound (0.08 g) which was converted the HCl salt.

1. concentrationconcentrated to dryness
2. additiontreated with ethanol (10 mL)
3. additiontreated with 6N HCl (3 mL)
4. temperaturerefluxed for 5 hours
5. concentrationconcentrated to dryness, Purification of the residue on silica gel (10:90:1 ethanol/methylene chloride/saturated ammonium hydroxide)