Classifications

• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
  • C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
  • C07F9/66—Arsenic compounds
  • C07F9/70—Organo-arsenic compounds
  • C07F9/74—Aromatic compounds

Definitions

• the present invention is for the manufacture of basic bismuth salts of aryl-arsinic acids, and has particular reference to the manufacture of the bismuth salt of N- phenyl-glycinamide-p-arsinic acid.
• the basic bismuth salts of aryl-arsinic acids possess therapeutic properties, and, appropriately prepared, are suitable for injection; and it has been found that in such salts the therapeutic properties of both bismuth and arsenic are advantageously combined, the toxicity of the products being generally of a low order.
• the method has a number of disadvantages. If solutions of equimolecular' proportions of the aforesaid type of reagents be mixed together at ordinary temperature, precipitation of the new compound is slow and incomplete, and the yield poor. With application of heat, precipitation is expedited, but without the production of a satisfactory yield. If the attempt be made to correct incomplete precipitation by leavingthe reaction mixture to stand, the precipitate frequently appears in the form of a gel, which is difficult to wash, and even in these circumstances, an' unsatisfactory yield of the new salt is obtained.
• the process of the present invention consists in an adaptation of the aforesaid process to the manufacture of basic bismuth salts of the type described, whereby the salts are obtained in substantial yield, and in a form readily adaptable to purification and to the preparation of therapeutic solutions.
• the manufacture of basic bismuth salts of arylarsinic acids is characterized by precipitating the solution of a bismuth salt with the solution of a salt of an aryl-arsinic acid un der application of heat in presence of a con siderable excess of the aryl-arsinic acid salt.
• the preferred type of bismuth salts with which to effect precipitation are salts of hydroxy-polybasic acids, of which tartaric acid is an example, such salts being conveniently employed in the form ofthe soluble double salts with such acids of bismuth and alkaline bases, as, for example, sodium-, or sodiumpotassium-, bismuth tartrate.
• the solution of a soluble bismuthyl salt of a hydroxy-polybasic acid such as tartaric acid
• a soluble bismuthyl salt of an aryl-arsinic acid may be added to the solution containing a substantial excess over the molecular equivalent of a soluble salt of an aryl-arsinic acid.
• an aqueous solution of an alkali bismuthyl tartrate such as sodium bismuthyl tartrate
• an aqueous solution of the sodium derivative of the aryl-arsinic acid in considerable excess over the quantity theoretically equivalent to the bismuthyl salt.
• the precipitated bismuth oxy-saltof the arsinie acid is washed and dried, preferably at a low temperature. It is advisable in most cases to separate the precipitate from the reaction liquor without undue delay in order to avoid undesirable change in condition of the product.
• the excess should not be below about 25 per cent, and may be as high as 80 per cent.
• the PHI' As in the case of the temperature factor, the PHI'.
• the reacting substances may be mixed together at the ordinary temperature, and the temperature then appropriately raisedand maintained as may be necessary to promote the reaction and the separation of a fine washable precipitate. If the temperature be too low, the precipitate tends to assume the form of avgel, while if the temperature at least 30 C.
• the precipitate may separate in too line a condition for satisfactory handlingf
• a temperature of 100 C. produces a precipitate so finely sub-divided as tomake Washing diflicult and protracted.
• the generally )referred temperature is one about C.
• Tendency to gel formation is generally observable up to a temperature of As Will be appreciated, a definite rule to meet all cases cannot be laid down as to'the degree of excess and the temperature; but the necessary adjustn'ient of these factors is attainable when it is borne in mind that the object in View is to produce a fine precipitate, which is yet sul'liciently. susceptible with reasonable facility to purification by Wash-- ing; and the limits given in illustration of the variation which may be made in the factors in question are those which have been found to be generally applicable with satis-. factory results.
• the precipitate should be separated Without delay, for a greater or less tendency to gel formation is displayed according to the length of time the reactionmixture is allowed to stand.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Inorganic Compounds Of Heavy Metals (AREA)

Applications Claiming Priority (1)

Publications (1)

Family

ID=10888031

Family Applications (1)

Country Status (3)

• 0
  • FR FR632834D patent/FR632834A/fr not_active Expired
  • BE BE338406D patent/BE338406A/xx unknown
• 1926
  • 1926-12-02 US US152307A patent/US1669542A/en not_active Expired - Lifetime

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