Excerpt: ...potash.8 1 Ann. 141, 131 (1867); 147, 43 (1868); 278, 210 (1893); Bud. soc. chim. (2) 40, 267 (1883); J. prakt. Chem. (1) 15, 129 (1838); Am. Chem. J. 15, 256 (1893); 20, 807 (1898). 2 J Chem. Soc. 99, 1251 (1911). 3 Ber. 8, 17 (1875). 4 Ber. 7, 1169 (1874); 10, 858 (1877). 5 Ber. 12, 329 (1879); Ann. chim. phys. (6) 1, 461 (1884). 6 Ber. 32, 1910 (1899). 7 Ber. 32, 1563 (1899). 8 Ber. 43, 3093 (1910). XII METHYL RED (o)HO2CC6H 4s NH2 + HNO2 + HCl- ( o)HO2CC6H4N2Cl + H2O (o) HO2CC6H4N2Cl + C6H5N(CH3)2- ( o)HO2CC6H4N = NC6H4N(CH3)2 + HCl Prepared by H. T. CLARKE and W. R. KIRNER. Checked by ROGER ADAMS and J. B. DAVIS. 1. Procedure TECHNICAL anthranilic acid (generally about 95 per cent pure) (685 g.) is dissolved in 1.5 l. of water and 500 cc. of concentrated hydrochloric acid (sp. gr. 1.17), by heating. The insoluble dark impurity present in small amounts is filtered off, and the filtrate is transferred to a 10-l. crock and chilled with stirring. It is then mixed with a mush of 2.5 kg. of ice and 750 cc. of concentrated hydrochloric acid. The crock is cooled externally with ice, and the contents stirred continuously. When the temperature reaches about 3'0, a filtered solution of 360 g. of sodium nitrite in 700 cc. of water is dropped in slowly, through a long capillary tube reaching below the surface of the liquid, until a faint but permanent reaction to starch potassium iodide paper is obtained; the temperature is kept between 3'0 and 5'0. This operation requires all but about 30 cc. of the nitrite solution and occupies one and a half to two hours. To the solution of the diazonium salt are now added 848 g. of dimethylaniline; this may be done rapidly, as the temperature does not rise appreciably. Stirring is continued for one hour, the temperature being kept at 5'0 Five hundred cc. of a filtered solution of 680 g. of crystallized sodium acetate diluted to 1200 cc. are then added, and the stirring continued for four hours. If a foamy solid rises...
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Add this copy of Organic Syntheses to cart. $36.96, new condition, Sold by Booksplease rated 4.0 out of 5 stars, ships from Southport, MERSEYSIDE, UNITED KINGDOM, published 2010 by Kessinger Publishing.
Add this copy of Organic Syntheses to cart. $36.96, new condition, Sold by Booksplease rated 4.0 out of 5 stars, ships from Southport, MERSEYSIDE, UNITED KINGDOM, published 2004 by Kessinger Publishing.
Add this copy of Organic Syntheses to cart. $43.48, good condition, Sold by Bonita rated 4.0 out of 5 stars, ships from Newport Coast, CA, UNITED STATES, published 2010 by Kessinger Publishing.
Add this copy of Organic Syntheses to cart. $43.48, good condition, Sold by Bonita rated 4.0 out of 5 stars, ships from Newport Coast, CA, UNITED STATES, published 2004 by Kessinger Publishing.
Add this copy of Organic Syntheses to cart. $57.17, new condition, Sold by Booksplease rated 4.0 out of 5 stars, ships from Southport, MERSEYSIDE, UNITED KINGDOM, published 2010 by Kessinger Publishing.
Add this copy of Organic Syntheses to cart. $57.17, new condition, Sold by Booksplease rated 4.0 out of 5 stars, ships from Southport, MERSEYSIDE, UNITED KINGDOM, published 2010 by Kessinger Publishing.
Add this copy of Organic Syntheses to cart. $60.29, good condition, Sold by Bonita rated 4.0 out of 5 stars, ships from Newport Coast, CA, UNITED STATES, published 2010 by Kessinger Publishing.
Add this copy of Organic Syntheses to cart. $63.87, good condition, Sold by Bonita rated 4.0 out of 5 stars, ships from Newport Coast, CA, UNITED STATES, published 2010 by Kessinger Publishing.
