反应详情

A solution of the product of Example IV (1.2 g, 0.005 m) and ethyl chloroformate (6.0 g, 0.0553 m) in acetone (20 ml) and H2O (50 ml) was treated with NaOH (0.1 ml aq. 30%) and the mixture stirred at room temperature for 15 min. The acetone was removed in vacuo and the aqueous residue cooled in an ice-bath. A solid formed and this was filtered, washed with water, and dried in vacuo. The crude product (1.0 g) was crystallized from methanol to afford the desired product; m.p. 80°-82° C.

1. customThe acetone was removed in vacuo
2. temperaturethe aqueous residue cooled in an ice-bath
3. customA solid formed
4. filtrationthis was filtered
5. washwashed with water
6. customdried in vacuo
7. customThe crude product (1.0 g) was crystallized from methanol