反应详情

Ethyl 2-[3-(2-thienyl)acrylamido]benzoate (150 mg, 0.50 mmol) prepared in Example 2 was dissolved in methanol (3 ml) while warming, and 1N-aqueous NaOH (1.8 ml, 1.80 mmol) was added dropwide under stirring. The mixture was stirred at 70° C. for 1 hour. After the reaction, methanol was removed, and the residue was treated with water under ice cooling and acidified (to pH 4) with 10% HCl. The precipitated solid were collected on a filter, washed with water, and dried to give white solids of the title compound (125 mg, yield, 92%), which were recrystallized from the mixed solvent of methanol and water. m.p., 215°-216° C.

1. temperaturewhile warming
2. stirringThe mixture was stirred at 70° C. for 1 hour
3. customwas removed
4. additionthe residue was treated with water under ice cooling
5. customThe precipitated solid were collected on a filter
6. washwashed with water
7. customdried