反应详情

Ethanol (500 ml) is added to (±)-4-(4-chlorophenyl)-6-ethoxycarbonyl-2,3,9-trimethyl-6H-thieno[3,2-f][1,2,4]triazolo-[4,3-a][1,4]diazepine-6-acetic acid (43 g), and the mixture is stirred at room temperature. 2N Sodium hydroxide (182 ml) is added and the mixture is stirred at 50° C. overnight. After the completion of the reaction, ethanol is distilled away, and the residue is adjusted to pH 4-5 with acetic acid. Then, the resulting mixture is stirred at 60° C. for 30 minutes and cooled to room temperature. The mixture is extracted with chloroform, and the organic layer is washed with saturated brine. The layer is dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The obtained crystals are recrystallized from chloroform-methanol to give 20 g of (±)-4-(4-chlorophenyl)-2,3,9-trimethyl-6H-thieno[3,2-f][1,2,4]triazolo-[4,3-a][1,4]diazepine-6-acetic acid, melting point 287°-290° C.

1. stirringthe mixture is stirred at 50° C. overnight
2. distillationis distilled away
3. stirringThen, the resulting mixture is stirred at 60° C. for 30 minutes
4. temperaturecooled to room temperature
5. extractionThe mixture is extracted with chloroform
6. washthe organic layer is washed with saturated brine
7. dry with materialThe layer is dried over anhydrous magnesium sulfate
8. concentrationconcentrated under reduced pressure
9. customThe obtained crystals are recrystallized from chloroform-methanol