反应详情

温度

70 °C

The crude product of Example 7 (17.2 g.). was dissolved in ethanol and 4.3 g. of gaseous hydrogen chloride were bubbled in. The reaction mixture was heated for 5 minutes at 70° C. Two crops of a solid, 12.4 g., m.p. 197°-220° C. (dec.), and 1.9 g., m.p. 224°-226° (dec.), were obtained. The two crops were combined and recrystallized from ethanol to obtain 11.8 g., m.p. 221°-232° C. (dec.). The mother liquors from each of the crystallizations and recrystallizations were combined; two additional crops, 4.9 g. (total), m.p. 193°-216° C. (dec.), were obtained therefrom. 11.5 g. of the combined crystalline materials were dissolved in water, excess sodium hydroxide solution was added, and the basic solution was extracted with methylene chloride. The methylene chloride extract was dried over anhydrous sodium sulfate, filtered and evaporated at reduced pressure. The residue was chromatographed on silica gel using ethyl acetate as the eluant. The major fractions were combined and recrystallized from acetone/pentane, 7.6 g., m.p. 118°-120° C. An analytical sample had a melting point of 120° C. A second crop (2.4 g.), m.p. 117°-119° C., was also obtained.

1. customof gaseous hydrogen chloride were bubbled in
2. custom, m.p. 224°-226° (dec.), were obtained
3. customrecrystallized from ethanol
4. customto obtain 11.8 g
5. customThe mother liquors from each of the crystallizations and recrystallizations
6. custom(total), m.p. 193°-216° C. (dec.), were obtained
7. extractionthe basic solution was extracted with methylene chloride
8. extractionThe methylene chloride extract
9. dry with materialwas dried over anhydrous sodium sulfate
10. filtrationfiltered
11. customevaporated at reduced pressure
12. customThe residue was chromatographed on silica gel
13. customrecrystallized from acetone/pentane, 7.6 g
14. customA second crop (2.4 g.), m.p. 117°-119° C., was also obtained