(
A) In
Pyrex 5-l. round-bottomed flask is placed a mixture of
500 g. (3.4 moles) of phthalic anhydride and
400 g. (444 cc., 6.6. moles) of 28 per cent aqueous ammonia. The flask is fitted with an
air condenser not less than 10 mm. in diameter and is then slowly heated with a free flame until the mixture is in a state of quiet fusion at a temperature of about 300° (Note
1). It requires about one hour before all the water has gone and about one and one-half to two hours before the temperature of the reaction mixture reaches 300° and the mixture is a homogeneous melt. It is advisable, during the heating, to shake the flask occasionally; some material sublimes into the condenser and must be pushed down with a
glass rod. The hot reaction mixture is now poured out into a
crock, covered with a paper to prevent loss by sublimation, and allowed to cool (Note
2). The product is practically pure without further treatment, and melts at
232–235° (Note
3). The yield is
470–480 g. (
95–97 per cent of the theoretical amount) (Note
4).
(
B)
Phthalimide may also be made by fusing
500 g. (3.4 moles) of phthalic anhydride and
500 g. (4.4 moles) of ammonium carbonate which has been previously ground in a
mortar. The subsequent procedure is the same as when aqueous
ammonia is used. Frequent shaking is necessary, and the sublimed material must be pushed back occasionally into the reaction flask. About two hours are required for completion.