反应详情

3-(4-Methanesulfonyl-phenoxy)-5-(2-methoxy-1-methyl-ethoxy)benzonitrile (0.1 g, 0.27 mmol) was dissolved in ethanol (1.0 ml) and charged to a 5 ml round bottomed flask equipped with a condenser. Water (0.2 ml, 11.1 mmol) was added, followed by sodium hydroxide (18.9M in water, 0.2 ml, 3.78 mmol). The reaction mixture was heated to reflux for 18 hours. The reaction mixture was cooled to room temperature, the solvent was evaporated in vacuo, the residue was partitioned between water (10 ml) and MTBE (10 ml) and the layers were separated. The aqueous phase was acidified to pH 1 with 2M HCl (2.5 ml, 5 mmol) and MTBE (10 ml) was added to extract the product. This MTBE extract was dried over MgSO4, and then evaporated in vacuo to give the title product as a white solid (0.1 g, 100% yield).

1. additioncharged to a 5 ml round bottomed flask
2. customequipped with a condenser
3. temperatureThe reaction mixture was heated
4. temperatureto reflux for 18 hours
5. customthe solvent was evaporated in vacuo
6. customthe residue was partitioned between water (10 ml) and MTBE (10 ml)
7. customthe layers were separated
8. additionwas added
9. extractionto extract the product
10. extractionThis MTBE extract
11. dry with materialwas dried over MgSO4
12. customevaporated in vacuo