摘要:
There is provided a method for the chlorination of a sucrose-6-acylate to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate, wherein said method comprises the following steps (i) to (v): (i) providing a first component comprising sucrose-6-acylate; (ii) providing a second component comprising a chlorinating agent; (iii) combining said first component and said second component to afford a mixture; (iv) heating said mixture for a heating period in order to provide chlorination of sucrose-6-acylate at the 4, 1′ and 6′ positions thereof; (v) quenching said mixture to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate; wherein at least one of said first component and said second component comprises a reaction vehicle, and said reaction vehicle comprises a tertiary amide; and wherein said mixture comprises a cosolvent during a least a portion of the heating period of step (iv), wherein said cosolvent comprises dimethylacetamide (DMAc).
摘要:
A waste treatment process and system is described, which finds application in dechlorinating carbohydrates and/or hydrolyzing dimethyl formamide and/or dimethyl formamide in a waste stream. The process includes treating the waste stream with base at a pH of from 11 to 14, and at a temperature of from 200 to 330° F.
摘要:
A chlorinating agent such as a chloroiminium species is used to remove or neutralize tertiary acetamide present as a contaminant in a tertiary formamide solvent. Tertiary formamide solvent purified or treated in this manner can be used as a reaction vehicle for the chlorination of sucrose-6-acylates, thereby improving the yields of the desired sucralose-6-acylate (an intermediate in the production of sucralose).
摘要:
There is provided a method for the chlorination of a sucrose-6-acylate to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate, wherein said method comprises the following steps (i) to (v): (i) providing a first component comprising sucrose-6-acylate; (ii) providing a second component comprising a chlorinating agent; (iii) combining said first component and said second component to afford a mixture; (iv) heating said mixture for a heating period in order to provide chlorination of sucrose-6-acylate at the 4, 1′ and 6′ positions thereof; (v) quenching said mixture to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate; wherein at least one of said first component and said second component comprises a reaction vehicle, and said reaction vehicle comprises a tertiary amide; and wherein said mixture comprises a cosolvent during a least a portion of the heating period of step (iv), wherein said cosolvent comprises perfluorooctane.
摘要:
The present invention relates to a method for the chlorination of a sucrose-6-acylate to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate wherein said method includes steps of: (i) combining the sucrose-6-acylate with a chlorinating agent in a reaction vehicle comprising a tertiary amide to afford a mixture; (ii) heating said mixture for a heating period in order to provide chlorination of sucrose-6-acylate at the 4, 1′ and 6′ positions thereof; and (iii) quenching the product stream of (ii) to produce a 4,1′,6′-trichloro-4,1′,6′-trideoxy-galactosucrose-6-acylate; wherein before said quenching, a portion of said tertiary amide is removed by extraction into a solvent in which said tertiary amide is at least partially soluble.
摘要:
A method of removing a carboxylic acid from a liquid including a tertiary amide solvent includes: A) forming an extraction medium including an acid-extracting tin species and an extraction solvent that is immiscible with the tertiary amide solvent; B) subsequently contacting the liquid with the extraction medium, forming a phase including a de-acidified tertiary amide solvent and a phase including the extraction solvent; and C) removing the phase including the extraction solvent, to afford a liquid including the de-acidified tertiary amide solvent. The acid-extracting tin species is one or more tin species obtainable by reaction of a di(hydrocarbyl)tin oxide with less than one equivalent of a carboxylic acid, tin species obtainable by reaction of a 1,3-diacyloxy-1,1,3,3-tetra-(hydrocarbyl)distannoxane with an aqueous base. A method of preparing a sucralose-6-acylate includes using the foregoing method to remove a carboxylic acid from a liquid including a tertiary amide solvent and the sucralose-6-acylate.
摘要:
A process for the purification of aqueous feed streams containing sucralose and/or sucralose 6-esters includes, providing an aqueous feed stream including the sucralose and/or sucralose 6-esters, concentrating the aqueous feed stream to form a concentrated aqueous feed stream containing at least 10 wt % total carbohydrates and extracting the concentrated aqueous feed stream with an organic solvent and producing an organic extract and an aqueous extract, in which the organic solvent is immiscible with water, and in which the carbohydrate preferentially passes into the organic extract.
摘要:
A chlorinating agent such as a chloroiminium species is used to remove or neutralize tertiary acetamide present as a contaminant in a tertiary formamide solvent. Tertiary formamide solvent purified or treated in this manner can be used as a reaction vehicle for the chlorination of sucrose-6-acylates, thereby improving the yields of the desired sucralose-6-acylate (an intermediate in the production of sucralose).
摘要:
A molten salt treatment system and process can include one or more tubular conduits flowably connected to a molten salt reactor, the tubular conduit containing concentrically within it a pipe or a shaft separated by an annular space therebetween, and one or more gas sources connected to feed gas into the annular space. The system may include a scrubbing device flowably connected to a molten salt reactor off-gas outlet to receive an off-gas, a first heating device configured to heat the effluent from the scrubbing device, and a filtering device flowably connected to receive the effluent from the heating device. An overflow conduit may be flowably connected to a molten salt reactor overflow outlet to receive molten salt therefrom and discharge the molten salt to a salt recovery vessel, and a blower or other gas mover may be connected to the molten salt reactor and the recovery vessel to prevent backflow of cold gases through the overflow outlet to the molten salt reactor.
摘要:
A method for the preparation of a sucrose-6-ester is disclosed. In a first step of the method, sucrose in a polar aprotic solvent is reacted with an organotin-based acylation promoter. The water of reaction is removed at a temperature that does not exceed about 80° C. In one aspect, the water is removed by distillation of part of the polar aprotic solvent at reduced pressure. In a second step, a carboxylic acid anhydride is added. In one aspect, the resulting reaction mixture is maintained at a temperature of 10° C. or less for a period of time sufficient to produce a sucrose-6-ester. The sucrose-6-ester can be converted to sucralose.