反应详情

温度

-30 °C

About 60 ml. of anhydrous ammonia were condensed into a flask containing 60 ml. of methylene chloride. The reaction mixture was maintained at a temperature not in excess of -30° C. under nitrogen and a solution of 50 g. of 2-t-butyl-5-methylisoxazolium perchlorate in 100 ml. of methylene chloride was added rapidly. The reaction mixture was allowed to come to room temperature and stirred for 4 days at room temperature. The methylene chloride was then removed at reduced pressure to obtain a gummy solid which was triturated with water to obtain a yellow solid. Recrystallization of the yellow solid from methanol/water yielded the product, m.p. 128°-129° C. Its spectra were identical with those of the product of Example 4(a).

1. customcondensed into a flask
2. additioncontaining 60 ml
3. customto come to room temperature
4. customThe methylene chloride was then removed at reduced pressure
5. customto obtain a gummy solid which
6. customwas triturated with water
7. customto obtain a yellow solid
8. customRecrystallization of the yellow solid from methanol/water
9. customyielded the product, m.p. 128°-129° C