PREPARATION OF NITROSYL CHLORIDE 251at 136-138°, with the flask immersed in an oil bath at 170-190°. About40-43 g. (56-60%) of product, m.p. 54-56°, is obtained. Recrystalli-zation from 35 cc. of methanol yields 38-40 g. (53-56%)bilarge yellowcrystals of 3-nitrobiphenyl melting at 58-59°. France, Heilbron, andHey6* obtained 7 g. of 3-nitrobiphenyl from 10 g. of m-nitroacetanilide.Nitrosation by Nitrosyl Chloride.The use of nitrosyl chloride in thepresence of sodium acetate8as a nitrosating agent shows much promise.Both the yield and the quality of the nitrosoacetylamines prepared bythis method are. superior to those resulting from the action of nitrousfumes, and the time required for the reaction is reduced from hours tominutes. Moreover, the reaction can be put on a quantitative basis,since a liquid (NOC1) or a solution of the liquid is employed. In this way,the detrimental results due to an excess of the nitrosating agent can be.avoided.
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