有没有合成过吲唑的? 这个化合物的合成方法如下:见organic syntheses, coll. vol. 3, p.660 (1955); vol. 20, p.73 (1940). 1. procedure to a solution of 55 g. (0.36 mole) of 2-amino-5-nitrotoluene (m.p. 129–132°) in 2.5 l. of glacial acetic acid in a 5-l. round-bottomed flask, provided with an efficient mechanical stirrer, is added all at once (note 1) a solution of 25 g. (0.36 mole) of sodium nitrite in 60 ml. of water. during this addition the temperature is not allowed to rise above 25° (note 2) . after the nitrite solution has been added, stirring is continued for 15 minutes to complete the diazotization. any yellow precipitate formed during the next few hours is filtered and discarded (note 3) . the solution is allowed to stand for 3 days at room temperature, and is then concentrated on the steam bath under reduced pressure (water pump) until spattering makes further evaporation impossible. two hundred milliliters of water is added to the residue, and the contents of the flask are washed into a small beaker where they are stirred to a smooth slurry. the product is filtered, washed thoroughly on the funnel with cold water, and dried in an oven at 80–90°. the crude material melts at 204–206° and weighs 47–57 g. (80–96%). it is purified by recrystallization from 650 ml. of boiling methanol using 5 g. of decolorizing charcoal. the recrystallized, pale yellow needles of 5-nitroindazole melt at 208–209°. the yield is 42–47 g. (72–80%) (note 4) . further recrystallization does not raise the melting point. 2. notes 1. if the sodium nitrite solution is added slowly, a considerable quantity of a yellow precipitate, presumably the diazoamino compound, is formed. 2. if the solution is cooled in an ice bath to 15–20° before addition of the nitrite solution, the temperature of the mixture will not rise above 25° during the diazotization. 3. this is presumably the diazoamino compound, insoluble in most organic solvents. it melts at about 200°. 1 4. the unsubstituted o -toluidine gives indazole itself, but the yield is very low (3–5%). 查看更多
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