File:Practical methods of organic chemistry (1901) (14585178567).jpg

Identifier: practicalmethods00gatt (find matches)
Title: Practical methods of organic chemistry
Year: 1901 (1900s)
Authors: Gattemann, Ludwig. (from old catalog)
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Publisher: (n.p.)
Contributing Library: The Library of Congress
Digitizing Sponsor: The Library of Congress

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, and on thisaccount find application in a very energetic, reaction; ether does notretard the reaction, but causes it to be more regular. At times, thereaction-mixture will not act, even on long standing. In this case,the reaction can frequently be started by a short heating, or the addi-tion of a few drops of ethyl acetate. Since the use of this compound,at times, causes a very stormy action, it is more advantageous to waitfor the reaction to begin spontaneously, even if a long time is necessary.In syntheses which are moderately difficult, the reaction-mixture, treatedwith a diluent, can be heated on the water-bath or in an oil-bath ;while, if the reaction takes place with great difficulty, the mixture,generally without dilution, must be heated in an oil-bath. In thelatter case, the reaction may be still further facilitated by heating underpressure of a mercury column. By this means, it is possible to heatthe reacting substances in an open vessel above their boiling-points.(Fig. 72.)
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Fig. 72. AROMATIC SERIES 253 19. REACTION: SULPHONATION OF AN AROMATIC HYDRO-CARBON (I) Example : (a) Benzenemonosulphonic Acid from Benzene andSulphuric Acid1(&) Sulphobenzide. Benzenesulphonchloride. Ben-zenesulphonamide (a) To 150 grammes of liquid fuming sulphuric acid, containingfrom 5-8 °lc of anhydride, placed in a 200 c.c. flask providedwith an air condenser, gradually add, with good shaking and cool-ing with water, 40 grammes of benzene ; before the addition of anew portion, always wait until the last portion, which at first floatson the surface of the acid, dissolves on shaking. The sulphona-tion requires about 10-15 minutes. The reaction-mixture is thenadded, with stirring, drop by drop, from a separating funnel, tothree to four times its volume of a cold, saturated solution ofsodium chloride contained in a beaker. In order that the solutionmay not be heated above the room temperature, the beaker isplaced in a large water-bath filled with ice-water. After sometime, but

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