• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
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  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Procedure for reducing ketones derived from continuous vitamin d and calcipotriol manufacturing process and corresponding use. Procedure for reducing ketones derived from vitamin d of general structure (V) or (VI) with borohydrides, where r1 and r2 may be the same or different and represent hydrogen or hydroxyl protecting groups, to give compounds of general structure (III) and (IV) or (VII) and (VIII), useful as intermediates for the synthesis of calcipotriol, where the reduction reaction is carried out in a continuous flow reactor. This procedure can be used as part of a calcipotriol manufacturing process. (Machine-translation by Google Translate, not legally binding)
    公开号:ES2620905A1
    申请号:ES201531925
    申请日:2015-12-29
    公开日:2017-06-30
    发明作者:Antonio BUXADÉ VIÑAS；Antonio Conchillo Teruel；Carlos Mola Soler
    申请人:Laboratorios Vinas SA；
    IPC主号:
    专利说明:

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    HPLC analysis: heptane / EBM 100: 15 at 2 ml / min and at 275 nm for reaction control.
    5 HPLC analysis: heptane / AcOEt 100: 4 at 1 ml / min and at 275 nm for impurity control. Example 4: Reduction of trans ketone (V) in various solvents
    10 Table 1 details other reactions carried out according to the method described in Example 3 and using the same proportions. The borohydride used is BH4Na. The solvents used to prepare solutions B and C are indicated. Solution A has always been prepared in tetrahydrofuran.
    15 Table 1
    Solvent - Solution B - Solution C Residual ketoneSaturated alcohol 24R, 24S24R allyl alcohol24S allyl alcohol24S / 24R ratio
    B: MeOH C: DMF 0.060.38 / 0.3458.540.60.69
    B: MeOH C: 0.05N NaOH 30.40.21 / 0.2540.827.40.67
    B: MeOH C: DMF / NaOH 30.60.17 / 0.2340.727.350.67
    B: EtOH C: DMF / NaOH 1.11.3755.841.80.75
    B: nPrOH C DMF / NaOH 0.620.955.043.20.785
    B: isoPrOH C: DMF / NaOH 24.051.3436.135.60.99
    B: DMF C: DMF / NaOH 6.80.28 / 0.3244.647.51,065
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    权利要求:
    Claims (1)
    [1]
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    同族专利:
    公开号 | 公开日
    ES2620905B1|2018-04-09|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    ES2234423A1|2003-12-05|2005-06-16|Laboratorios Viñas, S.A.|Preparation of vitamin D derivatives comprises reaction of a monohalogen vinyl derivative with e.g. metallic reagents|
    ES2411834A1|2011-12-30|2013-07-08|Laboratorios Viñas S.A.|Industrial process to obtain intermediates suitable for the synthesis of vitamin d analogues |
    法律状态:
    2018-04-09| FG2A| Definitive protection|Ref document number: 2620905 Country of ref document: ES Kind code of ref document: B1 Effective date: 20180409 |
    优先权:
    申请号 | 申请日 | 专利标题
    ES201531925A|ES2620905B1|2015-12-29|2015-12-29|Procedure to reduce ketones derived from vitamin D in continuous and procedure of manufacture of calcipotriol and corresponding use|ES201531925A| ES2620905B1|2015-12-29|2015-12-29|Procedure to reduce ketones derived from vitamin D in continuous and procedure of manufacture of calcipotriol and corresponding use|
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