反应详情

A 10 g (0.06 mole) quantity of the anhydride prepared in Example 1 was added in small portions to 120 mL conc. NH4OH. After the addition was completed, the mixture was heated to a gentle reflux and stirred for 4 hr. Upon cooling the reaction mixture, a yellow oil precipitated which solidified to a glass. Crystallization of the glass from isopropyl alcohol gave 8 g (80%) of crude product, m.p. 110°-120° C. (literature m.p. 115°-116°, Cf: N. S. Benica and C. O. Wilson, J. Am. Pharm. Assoc., 39, page 451-454 (1950)).

1. additionAfter the addition
2. temperaturethe mixture was heated to
3. temperaturea gentle reflux
4. temperatureUpon cooling the reaction mixture
5. customa yellow oil precipitated which
6. customCrystallization of the glass from isopropyl alcohol