Organic Syntheses by Unknown
page 81 of 106 (76%)
page 81 of 106 (76%)
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XX PHTHALIMIDE CO CO C6H4< >O + NH4OH--> C6H4< >NH + 2H2O CO CO CO CO 2C<6s Prepared by W. A. NOYES and P. K. PORTER. Checked by H. T. CLARKE and J. H. BISHOP. 1. Procedure IN a 5-l. round-bottom flask (Pyrex) is placed a mixture of 500 g. of phthalic anhydride and 400 g. of 28 per cent ammonium hydroxide. 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 300'0. It requires about one hour before all the water has gone and about one and a half to two hours before the temperature of the reaction mixture reaches 300'0 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. The product is practically pure without further treatment, and melts at 232-235'0. The yield is 470-480 g. (94-95 per cent of the theoretical amount). |
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