反应详情

A solution of the product of Example XXXVIII (3.0 g, 0.0117 m) and ethyl chloroformate (12.6 g, 0.117 m) in acetone (50 ml) and H2O (50 ml) was treated with NaOH (0.21 ml aq. 30%) and the mixture refluxed for 1 hr. The acetone was removed in vacuo and the aqueous residue cooled in ice-bath. A solid formed and this was filtered, washed with water, and dried in vacuo. The crude product (3.4 g) was crystallized from methanol (25 ml) to afford the desired product; m.p. 125°-127°.

1. temperaturethe mixture refluxed for 1 hr
2. customThe acetone was removed in vacuo
3. temperaturethe aqueous residue cooled in ice-bath
4. customA solid formed
5. filtrationthis was filtered
6. washwashed with water
7. customdried in vacuo
8. customThe crude product (3.4 g) was crystallized from methanol (25 ml)