Method for continuously preparing citalopram diol

    公开(公告)号:US11845710B2

    公开(公告)日:2023-12-19

    申请号:US17312635

    申请日:2019-12-02

    IPC分类号: C07C253/30

    CPC分类号: C07C253/30

    摘要: The present application relates to a method for citalopram intermediate citalopram diol. The method comprises: first mixing two Grignard reagents required for a reaction; then mixing the mixed Grignard reagents with a raw material 5-cyanophthalide in a temperature-controllable micromixer to obtain a reaction solution; then subjecting the reaction solution to the reaction by means of a reactor to obtain a citalopram diol reaction solution; and then performing operations such as quenching, concentration, extraction, acidification, and crystallization to obtain a qualified product. The citalopram diol provided in the present invention has good selectivity, high yield, high safety, safety and reliability, and little sewage discharge, and is suitable for industrial production.

    METHOD FOR CONTINUOUSLY PREPARING CITALOPRAM DIOL

    公开(公告)号:US20220024860A1

    公开(公告)日:2022-01-27

    申请号:US17312635

    申请日:2019-12-02

    IPC分类号: C07C253/30

    摘要: The present application relates to a method for citalopram intermediate citalopram diol. The method comprises: first mixing two Grignard reagents required for a reaction; then mixing the mixed Grignard reagents with a raw material 5-cyanophthalide in a temperature-controllable micromixer to obtain a reaction solution; then subjecting the reaction solution to the reaction by means of a reactor to obtain a citalopram diol reaction solution; and then performing operations such as quenching, concentration, extraction, acidification, and crystallization to obtain a qualified product. The citalopram diol provided in the present invention has good selectivity, high yield, high safety, safety and reliability, and little sewage discharge, and is suitable for industrial production.

    SUVOREXANT INTERMEDIATE AND PREPARATION METHOD THEREOF

    公开(公告)号:US20190040052A1

    公开(公告)日:2019-02-07

    申请号:US16073929

    申请日:2017-01-25

    IPC分类号: C07D413/14 C07D413/04

    摘要: The present invention relates to a synthesis process of suvorexant, novel compounds represented by formulas II, III, IV or V, or salts thereof for preparing suvorexant, and a method for preparing the intermediates. The preparation method uses a chiral starting material to synthesize chiral compounds represented by formulas II, III, IV or V, the compounds obtained being used for synthesizing the suvorexant. The preparation method has the advantages of simple operation, low cost, mild reaction conditions, simple post-treatment, easy to purify, high yield, high ee value for the product, and easy to industrialize. In the reaction route shown, R represents benzyl, allyl or 1-phenethyl, or optionally substituted benzyl at the 2 position to 6 position, such as 4-methoxybenzyl, 4-nitrobenzyl, 2-methylbenzyl, 4-chlorobenzyl or 3-fluorobenzyl.