反应详情

温度

20 °C

To a stirred solution of the product of step (b) in 1,4-dioxane (5 ml) was added 0.1M sodium hydroxide solution (5 ml) and the reaction was stirred at 20° C. for 4 hours. The reaction volume was reduced by 50% in vacuo and then partitioned between water (50 ml) and dichloromethane (50 ml). The aqueous layer was acidified to pH 1 by the addition of 2M hydrochloric acid and then extracted with dichloromethane (3×50 ml). The combined organic layers were dried over magnesium sulphate and the solvent was removed in vacuo to give the title compound as a white solid (30 mg).

1. custompartitioned between water (50 ml) and dichloromethane (50 ml)
2. additionThe aqueous layer was acidified to pH 1 by the addition of 2M hydrochloric acid
3. extractionextracted with dichloromethane (3×50 ml)
4. dry with materialThe combined organic layers were dried over magnesium sulphate
5. customthe solvent was removed in vacuo