Abstract:
Esters of gamma -chloroacetoacetic acid may be prepared by reacting diketene and chlorine in the presence of a low boiling organic solvent at temperatures of -10* to - 30* C. and esterifying the reaction product while maintaining the aforementioned temperatures. This process produces yields up to 87 percent of theoretical with product purity of 97 to 98 percent.
Abstract:
MALONIC ACID DINITRILE IS PREPARED BY REACTING ACETONITRILE AND CYANOGEN CHLORIDE IN THE GASEOUS PHASE AT TEMPERATURES FROM 740 TO 780*C. TEMPERATURES FROM 750* TO 760*C. WITH MOLAR RATIOS OF 1:1 TO 1:5 OF CYANOGEN CHLORIDE TO ACETONITRILE ARE PREFERRED. THE CRUDE MIXTURE CONTAINING MALONIC ACID DINITRILE MAY BE PURIFIED BY CONVERSION OF THE PRINCIPAL IMPURITIES TO EASILY SEPARABLE COMPOUNDS BY A DIELS-ALDER OR SELECTIVE HYDROGENATION REACTION.
Abstract:
Malonic acid dinitrile is prepared by reacting acetonitrile and cyanogen chloride in the gaseous phase at temperatures between 780* C. and 1,200* C. Yields exceeding 80 percent can be obtained and when the reactants flow through the reactor in a condition exceeding laminar flow and extending into turbulent flow, molar ratios of acetonitrile to cyanogen chloride of 4:1 and over are preferred with residence times at reaction temperatures of less than about 5 seconds.
Abstract:
NICOTINIC ACID AND OTHER CARBOXLIC ACIDS HAVING A PYRIDINE NUCLEUS MAY BE PREPARED BY THE OXIDATION OF ALKYL PYRIDINE AND COMPOUNDS IN THE PRESENCE OF 25-600% EXCESS NITRIC ACID AT TEMPERATURES OF 180-370*C. WITH PRESSURES OF 20-500 ATM. THE NITRIC ACID CONCENTRATION OF THE REACTION MIXTURE IS ADJUSTED TO 10-28% TO PRECIPITATE AS CRYSTALLINE HYDRONITRATE AND SEPARATED FROM THE MIXTURE. THE PH OF AN AQUEOUS SOLUTION OF THE PYRIDINE CARBOXYLIC ACID HYDRONITRATE IS ADJUSTED WITH THE BASIC STARTING MATERIAL TO THE ISOELECTRIC POINT OF THE SPECIFIC PYRIDINE CARBOXYLIC ACID TO PRECEPITATE THE SAME. THE CRYSTALLINE PRECIPITATION IS SEPARATED AND THE MOTHER LIQUORS ARE COMBINED AND RECYCLED AS THE STARTING MATERIAL AFTER ADJUSTMENT OF THE CONCENTRATIONS THEREIN.