Some derivatives of 4(or 5)-methyl-glyoxaline / by Arthur James Ewins.

  • Ewins, Arthur James.
Date:
[between 1910 and 1919?]
Catalogue details

Licence: In copyright

Credit: Some derivatives of 4(or 5)-methyl-glyoxaline / by Arthur James Ewins. Source: Wellcome Collection.

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    The dihydrochloride crystallises from absolute alcohol in colour¬ less, prismatic needles, melting at 231—232°: 0T295 gave 0'1732 C02 and 00801 H20. C = 36'5; H = 68. C6HnN3,2HCl requires 0 = 36*7; H = 6*6 per cent. This salt is anhydrous, very sparingly soluble in hot absolute alcohol, very readily so in cold water, and fairly readily so in cold methyl alcohol. With p-diazobenzenesulplionic acid in alkaline solution a reddish-yellow colour is produced. The aqueous solution of the salt is precipitated by mercuric chloride, the precipitate being soluble in dilute acids. The phosphotungstate of the base is readily soluble in hot water or in cold acetone. The dihydrobromide crystallises from absolute alcohol, on addition of dry ether, in stout, hexagonal prisms, melting at 212°: 0-1028 gave 0*1348 AgBr. Br = 55’8. C6HnN3,2HBr requires Br = 55‘8 per cent. 4(or b)-Methyl-5(or 4t)-methyla?mnomcthylglyoxali?ic, CI-VC-KH CH8-NH-CH2-C— This base was obtained by the action of methylamine on 4 (or 5)-methyl-5(or 4)-chloromethylglyoxaline. 0'5 Gram of 4(or 5)-methyl-5(or 4)-chloromethylglyoxaline was dissolved in a few c.c. of methyl alcohol, and the solution added drop by drop to 2’5 c.c. of an aqueous solution of methylamine, which was kept at a temperature of about 0°. The solution was then evaporated to dryness, the residue dissolved in a little water, and treated with a hot saturated aqueous solution of picric acid. The heavy, yellow oil which separated from the hot solution was collected, and from the filtrate on cooling the crystalline 4(or 5)-methigl-b (or k)-methyla minora ethyl glyoxaline dipicrate sepa¬ rated. It crystallises from water in prisms melting at 222°. Yield, 20 per cent, of theory: 0-1218 gave 0-1654 C02 and 0*0352 H20. 0 = 37-0; H = 32. 00944 „ 17*4 c.c. N2 (moist) at 16° and 764 mm. N = 21*6. C6H11N3,(C6IT307N3)2 requires 0 = 37*0; H = 29; N = 21*6 per cent. The dihydrochloride crystallises from absolute alcohol in stout prisms, melting at 246—247° : 0-1014 gave 0*1480 AgCl. 01 = 36-1. C6HnN3,2HCl requires 01 = 36’2 per cent.