反应详情

To a mixture of the acid of Example 1 (2.32 g, 6.5 mmol), 0-methylhydroxylamine hydrochloride (0.54 g, 6.5 mmol) and 1-ethyl-3-[3-(dimethylamino)propyl]carbodiimide (1.25 g, 6.5 mmol) in tetrahydrofuran (100 ml) is added triethylamine (2.0 ml, 2 equiv). After overnight stirring at room temperature, the solvent is removed and methylene chloride is added. This is followed by sequential washings with 0.05N hydrochloric acid and water (2x). After drying over magnesium sulfate, the solvent is removed to afford a crude solid which is recrystallized from ethyl acetate to afford a white crystalline solid, 0.6 g(24%), m.p. 162°-164° C.

1. customthe solvent is removed
2. additionmethylene chloride is added
3. washThis is followed by sequential washings with 0.05N hydrochloric acid and water (2x)
4. dry with materialAfter drying over magnesium sulfate
5. customthe solvent is removed
6. customto afford a crude solid which
7. customis recrystallized from ethyl acetate
8. customto afford a white crystalline solid, 0.6 g(24%), m.p. 162°-164° C.