Introduction to the study of organic chemistry : a text-book for students in the universitites and technical schools / by John Wade.

  • Wade, John.
Date:
1898
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Licence: Public Domain Mark

Credit: Introduction to the study of organic chemistry : a text-book for students in the universitites and technical schools / by John Wade. Source: Wellcome Collection.

    452/490 (page 430)
    CHAPTER XXXVIII [Estimation of Phosphorus.—As with sulphur. Phosphoric acid converted into magnesium pyrophosphate in usual manner.] Cacodyl.—In very small quant, by heating dry sodium acetate (£ centi- gram), with equal bulk white arsenic. Vapour poisonous and produces nausea. Zinc Ethyl.— (See chap. xiv.). Mercaptan.—9 grams ethyl sodium sulphate; 3 granu caustic soda Form mercury compound. PART 111 CHAPTER XXXIX [Benzene from Commercial Product.—Fractionate 50 c.c. “50%’,’ benzene from w.-b. Neglect residue boiling above 100°. Re-fractionate until fraction 79-81° obtained. Then freeze until m.-pt. constant. Take sp.-gr. (Benzene vapour, like ether very heavy and inflammable.)] Bromobenzene.—14 c.c. benzene (const, m.-pt.), 10 c.c. bromine, 5 gram iron filings. (Pass hydrogen bromide into 20 c.c. water and keep for chap, xlvii.; large bulb pipette just dipping under surface of water prevents passage backwards after air is expelled). In steam distillation ordinary llask may be substituted.for distilling flask; tilt to keep spray from con- denser. Wash with caustic soda before drying. Note b.-pt., sp.-gr., and halogen flame. Yield 70%. Nitrobenzene.—20 c.c. nitric, 20 c.c. sulphuric acid, 20 c.c. benzene. Pro- duct into beaker of cold water. Note b.-pt. and sp.-gr. Yield 80%. Sodium Benzene-Sulphonate.—40 c.c. benzene, 80 c.c. cone, acid or same qty. fuming acid. Sodium salt as iu chap. iv.; or by briue method (60 grams salt in minimum qty. of water; not so certain). Test for sulphur. Yield 70% . Benzene-Sulphonic Chloride.—10 grams sulphonate, 15 grams penta- chloride, 50 c.c. water. Distil off ether on w.-b., and chloride from test- tube over gauze. Note b.-pt. and odour. Prove sulphur. Hydrolyse two or three drops, and prove chlorine. Yield 60%. Benzene-Sulphonamide.—Use remainder of sulphonic chloride ; 10 grams carbonate per c.c. Recrystallise until m.-pt. sharp. Prove sulphur and nitrogen. Hydrolyse with caustic soda in test-tube, and prove ammonia. Yield 80%. CHAPTER XL Aniline.— 20 c.c. nitrobenzene, 120 c.c. cone, hydrochloric acid, 40 grams tin, 50 grams caustic soda powder in 200 c.c. water added until product grayish and fairly limpid. Steam distil from large flask. Collect yellow drops, dry with solid caustic soda, and pour off and distil from gauze. Shake water with T\;th its vol. of ether, and 5 grams caustic soda; separate. Repeat once. Dry mixed ethereal extracts with stick of soda, pour off, and distil off ether from w.-b. (no flame) and save ; then aniline from test tube over gauze. Note b.-pt. of both portions. Test. Yield 80%. Qualitative Tests for Aniline (p. 247).—Odour (alkali if necessary). Pure / liquid pptd. by dil. hydrochloric acid. Isocyanide. Mustard oil. Nitrogen and phenol with nitrite. Violet with bleaching soln. Blue with bichromate and cone, sulphuric acid. Acetanilide.—10 c.c. aniline; 10 c.c. glacial acid; four hours at least. (y Distil as with acetamide ; anilide passes over above 280°. Recryst. from hot water (filter hot) until m.-pt. const. Y'ield 90%. Hydrolysis of Acetanilide.—Boil 2 grams with 2 grams caustic soda and 20 c.c. water. Steam distil aniline and test. Distil residue with dil. sul- phuric acid and prove acetic acid.