反应详情

温度

100 °C

To a solution of 2-(4-{[(3-tert-butoxycarbonylmethoxy-benzyl)-(pyridine-3-sulfonyl)-amino]-methyl}-phenyl)-2-methyl-propionic acid ethyl ester (138 mg, 0.237 mmol) in MeOH (5 mL) was added aqueous NaOH (2N, 0.36 mL, 0.72 mmol). The reaction was heated at 100° C. for 1 h and was cooled to room temperature. The reaction was concentrated in vacuo and was diluted with water and EtOAc. The pH was adjusted to about 5 with 1N HCl. The aqueous solution was washed with EtOAc (3×). The combined organic solutions were dried (MgSO4), filtered, and concentrated. Sodium chloride was added to the aqueous solution and the solution was washed with EtOAc (3×). The combined organic solutions were dried (MgSO4), filtered, and concentrated. The combined title compound (104 mg) was used in the next step without further purification. MS 527 (M+1).

1. temperaturewas cooled to room temperature
2. concentrationThe reaction was concentrated in vacuo
3. additionwas diluted with water and EtOAc
4. washThe aqueous solution was washed with EtOAc (3×)
5. dry with materialThe combined organic solutions were dried (MgSO4)
6. filtrationfiltered
7. concentrationconcentrated
8. additionSodium chloride was added to the aqueous solution
9. washthe solution was washed with EtOAc (3×)
10. dry with materialThe combined organic solutions were dried (MgSO4)
11. filtrationfiltered
12. concentrationconcentrated
13. customwas used in the next step without further purification