The very thick paste is treated with 80 cc. sodium hydroxide solution (40° Вё), and the mixture is heated to 80°C. to form a clear solution. In the course of 15 minutes 80 grams of powdered sodium hydrosulfite, is added to this solution with stirring at a temperature of 80-90°. (The reduction should be carried […]
Архивы рубрики ‘DYE CHEMISTRY’
Preparation of the Аго Dye
A solution is made of 18.6 grams (0.2 mole) of aniline in a mixture of 45 cc. concentrated hydrochloric acid (21° Be) and 45 cc. water. The solution is cooled to 0°C. in an ice-salt bath, and a solution of 14 grams of sodium nitrite in 40 cc. water is added slowly with good stirring […]
Aminophenob4,6-disulfonic Acid from Phenol
(1) Nitrophenoldisulfonic Acid. 94 grams of pure phenol is melted at 50° in an iron sulfonation kettle, and 300 grams of 100 per cent sulfuric acid is added to it, with good stirring, over a period of 10 minutes. The mixture is heated to 100°C. for 1 hour, then cooled to 50°, and 300 grams […]
Picramic Acid
OH OH o2&/no2 o2n/Ni 1 1 —> / / no2 no2 In a glass or iron container of at least 2.5-Iiter capacity, a solution of 10 grams of picric acid and 10 grams of 35 per cent sodium hydroxide in 600 cc. water is heated to 55°C., and to this is added, with vigorous stirring […]
Trinitrophenol (Picric Acid)
OH OH OH SO, H NO* Phenol Disulfonic acid Trinitrophenol In a glass’, iron, or porcelain sulfonation vessel, 94 grams of phenol of the highest quality is heated to 100°C., and 300 grams of 100 per cent sulfuric acid is added with stirring at such a rate that the temperature remains below 110°. The mixture […]
Alkylation of Nitrophenols
Nitrophenols are converted to their ethers by the general method outlined below. One mole of the phenol is dissolved in 400 cc. water containing 1 mole of sodium hydroxide and 80 grams of soda ash. To this solution is added 500 cc. 90 per cent alcohol (ethyl or methyl) and the whole is cooled to […]
Derivatives of Phenol
o — and p-Chlor о phenol from Phenol OH OH OH Cl The two isomers are prepared by the method of Dubois (1866), by the action of excess sulfuryl chloride on phenol, and are separated by fractional distillation. In a 1-liter three-necked flask fitted with a stirrer, thermometer, dropping funnel, and gas exit tube, is […]
Aceto acetanilide
+ 2 NasSOj -f гН,0 S03Na ONa In the tray of a vacuum baking oven (Fig. 30, page 181), 32 grams (0.8 mole) of sodium hydroxide is dissolved in 20 cc. water by heating to 200° C., then 28.2 grams (0.1 mole) of sodium benzene-m-disulfonate (preceding preparation) is added and the mixture is stirred to […]
Diphenylamine from Aniline and Aniline Salt
In an enameled autoclave having an enameled thermometer tube, 93 grams of aniline and 93 grams of aniline hydrochloride are heated for 20 hours at 230°C. The pressure rises to about 6 atmospheres. If there is no enameled thermometer tube, the pressure is brought to this point, and the temperature of the oil bath is […]
. Tetramethyl-p, p’-diaminobenzophenone (Michler Ketone)
The condensation of dimethylaniline with phosgene yields, besides the p, p’ product, considerable quantites of the o, o’ and o, p’ compounds. The phosgene necessary for the reaction is taken from a phosgene cylinder,[27] and a small excess of dimethylaniline is used in order to be sure that all of the hydrogen chloride formed is […]