Abstract:
NEW MATERIAL:The compound of formula (R is 2-3C mononitratoalkyl or dinitratoalkyl). EXAMPLE:Acetoacetic acid 2-nitratoethyl ester. USE:Synthetic raw material of a dihydropyridine derivative useful as a remedy for coronary vessel circulation disorder, hypertension, etc. PROCESS:The compound of formula can be prepared by reacting a diketene with an alcohol of formula HO-R in the presence of a basic catalyst such as triethylamine, sodium acetate, etc.
Abstract:
The present invention relates to a process for preparing hexanoic acid, 6-(nitrooxy)-, (1S,2E)-3-[(1R,2R,3S,5R)-2-[(2Z)-7-(ethylamino)-7-oxo-2-hepten-1-yl]-3,5-dihydroxycyclopentyl]-1-(2-phenylethyl)-2-propen-1-yl ester of formula (I). In accordance with the present invention, the compound (I) can be efficiently prepared with high purity by coupling bimatoprost in a boronate protected form with 6-(nitrooxy)hexanoyl chloride and removing the boronate protecting group. The invention also relates to a process for the preparation of 6-(nitrooxy) hexanoic acid having a HPLC purity equal to or greater than 99% and containing an amount of 6- {[6-(nitrooxy)hexanoyl]oxy}hexanoic acid (compound (IXa) equal to or lower than 0.2%.
Abstract:
The invention relates to a process for the preparation of ω-nitroxyC 3-1 0 alkane-1-ols comprising the nitration of an α,ω-C 3-10 alkanediol with a nitration agent, optionally in the presence of a nitrite trapping agent, characterized in that the nitration agent is a mixture consisting of 50 to 75 wt.-% of nitric acid in water wherein the nitric acid is used in an amount selected in the range from 0.5 to 5 mol equivalents based on the α,ω--C 3-10 alkanediols, and wherein the nitration is carried out at a temperature selected in the range from 65 - 100°C.
Abstract:
A process for synthesizing isooctyl nitrate in a continuous flow reactor comprises flowing a H2SO4-HNO3 mixture within a flow reactor, flowing isooctyl alcohol into said flow reactor so as to mix the isooctyl alcohol with the H2SO4-HNO3 mixture and produce a reaction mixture stream flowing in said reactor, maintaining the reaction mixture stream flowing in said flow reactor at a reaction temperature within in the range -10° to 35°C inclusive, and wherein the residence time of the reaction mixture stream in the flow reactor is greater than or equal to 5 seconds and less than or equal to 40 seconds, and wherein the H2SO4 of the H2SO4-HNO3 mixture is H2SO4 having a concentration of in the range of 85 to 95% inclusive, more desirably 88 to 92% inclusive, most desirably of 90%.
Abstract translation:在连续流动反应器中合成硝酸异辛酯的方法包括使流动反应器内的H 2 SO 4 -HNO 3混合物流动,将异辛醇流入所述流动反应器中,以将异辛醇与H 2 SO 4 -HNO 3混合物混合并产生流动的反应混合物流 在所述反应器中,保持反应混合物流在所述流动反应器中流动的反应温度在-10℃至35℃的范围内,并且其中反应混合物流在流动反应器中的停留时间大于或等于 至5秒且小于或等于40秒,并且其中H 2 SO 4 -HNO 3混合物的H 2 SO 4为浓度为85-95%(含)的H 2 SO 4,更优选为88-92%,最优选为90 %。
Abstract:
The invention relates to a method for the production of liquid nitrate esters, e.g. nitro-glycerine, wherein an alcohol is esterified by means of nitrating acid and the reaction takes place in one or several microreactors.
Abstract:
A process for the preparation of compounds of formula: HO-A-ONO 2 (I) wherein A is a C 2 -C 6 alkylene chain by nitration of the corresponding alkanediols with "stabilised" nitric acid is herein disclosed. The process is safer to operators and allows to obtain advantageous yields on an industrial scale.
Abstract:
A method for preparing a nitrate ester is provided. The method includes providing a first solution including a compound (which has at least one hydroxyl group) and a carboxylic acid having 2-5 carbon atoms; providing a second solution including nitric acid, acetic anhydride, and acetic acid; and transferring the first solution and the second solution to a microreactor, obtaining a nitrate ester after a residence time. In particular, the ratio of the weight of nitric acid to the total volume of the acetic anhydride and acetic acid is 1:1 to 1:3.5. The ratio of the molar amount of nitric acid to the hydroxyl group equivalent of the compound is from 1:1 to 15:1.
Abstract:
Process for the production of a chemical compound from a carbon dioxide starting material, comprising the steps of a) providing a feed stream consisting mainly of carbon dioxide; b) electrolyzing in an electrolysis stage the carbon dioxide in the feed stream to a first gas stream containing carbon monoxide and a second gas stream containing oxygen, wherein the molar ratio between carbon monoxide and oxygen is about 1:0.5 in an electrolysis stage; c) adjusting the composition of the first gas stream or the second gas stream or both gas streams to include carbon dioxide, either by operating at less than full conversion of CO2 or by sweeping one or both gas streams with a gas containing CO2 or by at some stage between the electrolysis cell and the oxidative carbonylation reactor diluting one or both gas streams with a gas containing CO2; all while maintaining an overall molar ratio of carbon monoxide to oxygen of about 1:0.5; and d) introducing the first and second process stream into a reaction stage and reacting the first and second process stream combined or in succession with a substrate to the chemical compound by means of an oxidative carbonylation reaction with the carbon monoxide and oxygen contained in the process feed stream.
Abstract:
A process for the continuous production of a compound of Formula (II), HO—R1—ONO2 (II) wherein R1 is a straight chain alkyl radical having from 3 to 6 carbon atoms, in a two-phase solvent system, comprising contacting a compound of Formula (I), HO—R1—OH (I) wherein R1 is as defined above, with nitric acid in the presence of a first solvent, wherein the compound of Formula (II) is continuously extracted into a second solvent, and the reaction is carried out in a mixing microreactor which provides a power loss of at least 1.3 times the power loss provided under identical conditions by a circular cross-section straight-channel microreactor having an internal diameter equal to the average hydraulic diameter of the mixing microreactor and a length equal to the length of the mixing microreactor.