. Journal. v driven, and 1200 grms. (1280 ) ofcommercial diethylaniline (containing 5—10%of monoethylamline) is added. The temperature 148 PRICE, BRAZIER & WOOD—PREPARATION OF DIETHYLAMINE. [Feb. 15, 1916. is then reduced to about 5 O. by the judiciousaddition of ice. A sohiton of GW j^rins. of98—1>0^\, soiliuiu nitrite, that is. 10\, excess, in1400 of water is tlieu added slowly, the timer«—S C. by the addition of ice fromtime to time, this tt^mperature beini; more satis-factory than 0 C. When all the nitrite- has beenadded, the stirring is continued for —;>0 minutes,and the
. Journal. v driven, and 1200 grms. (1280 ) ofcommercial diethylaniline (containing 5—10%of monoethylamline) is added. The temperature 148 PRICE, BRAZIER & WOOD—PREPARATION OF DIETHYLAMINE. [Feb. 15, 1916. is then reduced to about 5 O. by the judiciousaddition of ice. A sohiton of GW j^rins. of98—1>0^\, soiliuiu nitrite, that is. 10\, excess, in1400 of water is tlieu added slowly, the timer«—S C. by the addition of ice fromtime to time, this tt^mperature beini; more satis-factory than 0 C. When all the nitrite- has beenadded, the stirring is continued for —;>0 minutes,and then the solution si|ihoned olT into a ^lassholder. B. which is routrhly graduated in solid nitroso-hydrochloride sepai-ates out inany quantity, enough water is added to dissolveit. before siphoning takes pliwe. The volumeof the solution thus obtained is about 10 fitted between the delivery tube and the con-densers, for retaining any tarry matter whichmay ilistil over. It is heated on a water bath,and is littcd with a siplmii tulic (not shown in thediagram) for emptying il from time to time. About 500 of the solution of the nitroso-compound is now run in from B. when the crudedietliylamine immediately commences to distilover, and is collei-ted_ in the receiver, H. Anyescaping vapour is absorbed by the trap, K, wliiciiis lilled with small glass tiibes, moistened withiiydrocldoiic acid, and opens into a jar containinghydrochloric acid solution (1:1). The li(|uiddropping from the end of tlie IJavies condenseris yellow in colour and shovdd lie nuite soon as it becomes milky, more solution (,)00 )of the nit Ioso-compound is rim into the Ian. Thislatter solution shoidd be run in ipuckly, and notslowly, otherwise decomposition occurs. Whenthe distillation is proieeding smoothly, the remain-ing sodium hydroxide sohition in 1) can be
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Keywords: ., bookcentury1800, bookdecade1880, booksubjectchemist, bookyear1882
