PROCESS FOR THE PREPARATION OF A NITRIC OXIDE DONATING PROSTAGLANDIN ANALOGUE

    公开(公告)号:WO2022167070A1

    公开(公告)日:2022-08-11

    申请号:PCT/EP2021/052553

    申请日:2021-02-03

    Applicant: NICOX S.A.

    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%.

    CONTINUOUS SYNTHESIS OF ISOOCTYL NITRATE IN A FLOW REACTOR
    325.
    发明申请
    CONTINUOUS SYNTHESIS OF ISOOCTYL NITRATE IN A FLOW REACTOR 审中-公开
    在流动反应器中连续合成硝酸异氰酸酯

    公开(公告)号:WO2015134703A1

    公开(公告)日:2015-09-11

    申请号:PCT/US2015/018876

    申请日:2015-03-05

    CPC classification number: C07C201/02 C07C203/04

    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 %。

    METHOD FOR PREPARING NITRATE ESTER
    328.
    发明申请

    公开(公告)号:US20200140372A1

    公开(公告)日:2020-05-07

    申请号:US16413322

    申请日:2019-05-15

    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.

    Process for the production of chemical compounds from carbon dioxide
    329.
    发明授权
    Process for the production of chemical compounds from carbon dioxide 有权
    从二氧化碳生产化学化合物的方法

    公开(公告)号:US09273020B2

    公开(公告)日:2016-03-01

    申请号:US14394508

    申请日:2013-04-11

    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 translation: 用于从二氧化碳原料生产化合物的方法,包括以下步骤:a)提供主要由二氧化碳组成的进料流; b)在电解阶段中将进料流中的二氧化碳电解成含有一氧化碳和含有氧的第二气流的第一气流,其中在电解阶段一氧化碳和氧之间的摩尔比为约1:0.5; c)调节第一气流或第二气流或两种气流的组成以包括二氧化碳,或者通过以少于二氧化碳的全部转化率进行操作,或者通过用含有CO 2的气体或通过在 在电解池和氧化羰基化反应器之间的某个阶段,用含CO 2的气体稀释一种或两种气流; 同时保持一氧化碳与氧的总摩尔比为约1:0.5; 和d)将第一和第二工艺流引入反应阶段,并通过与该方法中所含的一氧化碳和氧气进行氧化羰基化反应,将第一和第二工艺流与底物组合或连续地与化学化合物反应 饲料流。

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