合成Diazald的?铨
我想在??室?用Diazald 甲醇制取重氮甲烷。但是N-甲基-N-亚硝基对甲苯磺酰胺(diazald) （CAS No 80-11-5 ）偕不到。
所以得自己制取，在
[url=http://www.orgsyn.org/]http://www.orgsyn.org/[/url]
上面找到如下合成方法：
1. Procedure
A total of 320 g. (1.68 moles) of p-toluenesulfonyl chloride (Note 1) is divided into three portions of 190, 90, and 40 g.; and a solution of alkali is prepared by dissolving 70 g. of sodium hydroxide in 70 ml. of water with cooling. The 190-g. portion of the sulfonyl chloride is added with swirling during about 5 minutes to 210 ml. (2.1 moles) of 33% aqueous methylamine (or 174 ml. of the 40% solution) contained in a 1-l. round-bottomed flask. The mixture is allowed to heat up to 80?90° in order to maintain the sulfonylmethylamide (m.p. 78°) in a molten condition (Note 2). After all this portion of the sulfonyl chloride has been added, the mixture is shaken vigorously. Boiling is prevented by mild cooling with water in order to avoid an excessive loss of methylamine.
As soon as the mixture has become acidic (Note 3), as indicated by testing a drop on litmus paper, 50 ml. of the 50% sodium hydroxide solution is added carefully with swirling. This is followed immediately by gradual addition of the 90-g. portion of the sulfonyl chloride as before. When the mixture has again become acidic (Note 3), 25 ml. of the sodium hydroxide solution is added, followed by the final 40 g. of the sulfonyl chloride. After the mixture has again become acidic, the remainder of the sodium hydroxide solution is added. The liquid phase of the final mixture should be alkaline (Note 4).
After the walls of the flask have been rinsed with a little water, the reaction is completed by heating the mixture, consisting of two layers and a precipitate of sodium chloride, on a steam bath for 15 minutes with vigorous mechanical stirring. The hot reaction mixture (Note 2) and (Note 5) is then poured into 1.5 l. of glacial acetic acid contained in a 5-l. round-bottomed flask, and the smaller flask is rinsed clean with 250 ml. of acetic acid (Note 6). The solution is cooled in an ice bath to about 5° (Note 7) and stirred mechanically as a solution of 124 g. (1.8 moles) of sodium nitrite in 250 ml. of water is added from a dropping funnel during about 45 minutes. The temperature of the mixture is kept below 10°, and stirring is continued for 15 minutes after addition is complete. During the reaction, the nitroso compound separates as a yellow crystalline product.
One liter of water is added to the mixture; then the precipitate is separated by suction filtration, pressed on the funnel, and washed with about 500 ml. of water. The product is transferred to a beaker, stirred well with about 500 ml. of cold water, then filtered and washed again on the funnel. This process is again repeated if necessary to remove the odor of acetic acid. After drying to constant weight in a vacuum desiccator over sulfuric acid, the product melts in the range between 55° and 60° (Note 8). The yield is 306?324 g. (85?90%) (Note 9) and (Note 10).
--------------------------------------------------------------------------------------
???铨：
呃??量?我?真大了?，我把所有的原料用量?少到1/5行不行？
页:
[1]