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    METHOD OF PREPARING ALKYL PHOSPHATE COMPOUND BASED ON MICRO-REACTION SYSTEM
    1.
    发明申请
    METHOD OF PREPARING ALKYL PHOSPHATE COMPOUND BASED ON MICRO-REACTION SYSTEM 有权

    公开(公告)号：US20250163084A1

    公开(公告)日：2025-05-22

    申请号：US19031731

    申请日：2025-01-18

    Applicant: Jiangxi Normal University ,  Fudan University

    Inventor： Fener CHEN ,  Xianjing ZHENG ,  Chang LIU ,  Yiqun TIAN ,  Yajiao ZHANG ,  Li WAN ,  Chunxue PENG ,  Songlin ZHENG ,  Liangchuan LAI

    IPC: C07F9/50 ,  B01J19/00 ,  C07F9/46

    Abstract: A method of preparing an alkyl phosphate compound based on a micro-reaction system. The micro-reaction system includes a feed pump, a first micro-mixer, a second micro-mixer, a first micro-channel reactor, a second micro-channel reactor and a back-pressure device, where the first micro-mixer, the second micro-mixer, the first micro-channel reactor, the second micro-channel reactor and the back-pressure device are sequentially connected. The method includes the following steps. An alkylamine compound and an acid-binding agent are simultaneously fed to a first micro-mixer for mixing and then to the first micro-channel reactor for pre-reaction to obtain a pre-reaction solution. The pre-reaction solution and a phosphate or phosphite are simultaneously fed to the second micro-mixer for mixing to obtain a first reaction mixture. The first reaction mixture is fed to the second micro-channel reactor to carry out a condensation reaction under a back pressure condition and is concentrated to obtain the final product.

    FULL CONTINUOUS SYNTHESIS DEVICE AND METHOD FOR METRONIDAZOLE
    3.
    发明公开
    FULL CONTINUOUS SYNTHESIS DEVICE AND METHOD FOR METRONIDAZOLE 审中-公开

    公开(公告)号：US20240270696A1

    公开(公告)日：2024-08-15

    申请号：US18625925

    申请日：2024-04-03

    Applicant: Fudan University

    Inventor： Fener CHEN ,  Minjie LIU ,  Li WAN ,  Yajiao ZHANG ,  Dang CHENG

    IPC: C07D233/94 ,  B01J19/00

    CPC classification number: C07D233/94 ,  B01J19/006 ,  B01J19/0066 ,  B01J19/0093 ,  B01J2219/00033 ,  B01J2219/00768 ,  B01J2219/00783 ,  B01J2219/00864 ,  B01J2219/00867 ,  B01J2219/00889

    Abstract: A full continuous synthesis method of metronidazole is provided. An aqueous glyoxal solution, an aqueous acetaldehyde solution and aqueous ammonia are mixed and reacted to produce a 2-methylimidazole-containing reaction mixture, which is mixed with a nitric acid solution and then reacted in the presence of concentrated sulfuric acid to obtain a 2-methyl-5-nitroimidazole-containing reaction mixture. The 2-methyl-5-nitroimidazole-containing reaction mixture is divided by a splitter, such that one part is used to replace concentrated sulfuric acid, and the other part is mixed with formic acid, and undergoes a ring-opening reaction with ethylene oxide to obtain a metronidazole solution. The metronidazole solution is adjusted to pH 2-6 and filtered to obtain a filtrate, which is adjusted to pH 8-14 and filtered to obtain a crude product. The crude product is subjected to decoloring, crystallization, filtration and drying to obtain pure metronidazole with a purity greater than 99.9%.

    FULL CONTINUOUS-FLOW PREPARATION METHOD OF (+)-BIOTIN
    4.
    发明公开
    FULL CONTINUOUS-FLOW PREPARATION METHOD OF (+)-BIOTIN 审中-公开

    公开(公告)号：US20230183260A1

    公开(公告)日：2023-06-15

    申请号：US18166906

    申请日：2023-02-09

    Applicant: Fudan University

    Inventor： Fener CHEN ,  Dang CHENG ,  Jiale WU ,  Meifen JIANG ,  Li WAN ,  Jiaqi WANG

    IPC: C07D495/04 ,  B01J19/00

    CPC classification number: C07D495/04 ,  B01J19/0093 ,  B01J2219/00867 ,  B01J2219/00033

    Abstract: A full continuous-flow preparation method of (+)-biotin, including: subjecting a cyclic anhydride and a chiral biphenyl propylene glycol to asymmetric ring-opening reaction to produce a first intermediate, which undergoes selective reduction with a borohydride and cyclization with an inorganic mineral acid to produce (3aS, 6aR)-lactone; subjecting the (3aS, 6aR)-lactone and a sulfenylating reagent to sulfenylation to produce (3aS, 6aR)-thiolactone, which undergoes Fukuyama coupling with a zinc reagent in the presence of a palladium catalyst and elimination reaction in the presence of an inorganic mineral acid to produce an alkenyl valerate compound; subjecting the alkenyl valerate compound to reduction in the presence of a Pd/C catalyst to produce a valerate ester, which undergoes hydrolysis to produce a valeric acid salt; and subjecting the valeric acid salt to debenzylation in the presence of an inorganic mineral acid to produce the target product (+)-biotin.

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