Process for the production of vasicine
    3.
    发明授权
    Process for the production of vasicine 失效
    生产vasicine的过程

    公开(公告)号:US06676976B2

    公开(公告)日:2004-01-13

    申请号:US10104765

    申请日:2002-03-21

    CPC classification number: C07D487/04

    Abstract: The present invention relates to an improved process for the production of vasicine of formula (1) from the Adhatoda vasica, said process comprising the steps of: extracting the dried and pulverized leaves with an alcoholic extract at an ambient temperature, concentrating the alcoholic extract to obtain a concentrated extract, treating and stirring extract with an aqueous organic acid for 2-24 hours, extracting the acid solution of with an organic solvent, separating the organic layer and aqueous acidic layer, basifying the aqueous acidic solution with a base, extracting the basified solution with an organic solvent, separating the organic layer, drying and filtering, evaporating the organic layer to obtain an amorphous residue, and treating the amorphous residue with an organic solvent or mixture of organic solvents to obtain vasicine.

    Abstract translation: 本发明涉及一种用于从Adhatoda vasica生产式(1)的维生素的改进方法,所述方法包括以下步骤:在室温下用醇提取物萃取干燥和粉碎的叶子,将醇提取物浓缩 获得浓缩提取物,用有机酸水溶液处理和搅拌提取物2-24小时,用有机溶剂萃取酸溶液,分离有机层和酸性水层,用碱将酸性水溶液碱化,提取 碱性溶液与有机溶剂分离,分离有机层,干燥和过滤,蒸发有机层,得到无定形残渣,用有机溶剂或有机溶剂混合物处理无定形残余物,得到vasicine。

    Process for the preparation of maltol from plants belonging to the genus Abies
    4.
    发明授权
    Process for the preparation of maltol from plants belonging to the genus Abies 失效
    从属于Abies属的植物制备麦芽酚的方法

    公开(公告)号:US06384246B1

    公开(公告)日:2002-05-07

    申请号:US09792030

    申请日:2001-02-26

    CPC classification number: C07D309/40

    Abstract: A process has been developed for production of a food flavoring compound maltol which comprises (a) extracting the dried and pulverized leaves of the plants belonging to the genus Abies with an alcohol at 20-40° C. and concentrating the solvent to obtain an alcoholic extract, (b) adsorbing the alcoholic extract with an adsorbent and drying the adsorbed material at a temperature ranging between 20-50° C., (d) partitioning of the adsorbed material between selected solvents consisting of aliphatic hydrocarbon and chlorinated solvent successively, (d) concentrating the chlorinated solvent to a residue and crystallizing it from a suitable organic solvent or mixtures of such solvents to get pure maltol.

    Abstract translation: 已经开发了用于生产食品香料化合物麦芽酚的方法,其包括(a)在20-40℃下用醇在20-40℃下提取属于Abies属的植物的干燥和粉碎的叶子并浓缩溶剂以获得酒精 提取物,(b)用吸附剂吸附醇提取物并在20-50℃的温度范围内干燥吸附的材料,(d)连续地将由脂族烃和氯化溶剂组成的选定溶剂之间的吸附材料分配(( d)将氯化溶剂浓缩至残余物并将其从合适的有机溶剂或这些溶剂的混合物中结晶得到纯的麦芽酚。

    Process for the production of (−) 3,4-divanillyl tetrahydrofuran
    5.
    发明授权
    Process for the production of (−) 3,4-divanillyl tetrahydrofuran 失效
    生产( - )3,4-二苯乙烯基四氢呋喃的方法

    公开(公告)号:US06372922B1

    公开(公告)日:2002-04-16

    申请号:US09818278

    申请日:2001-03-27

    CPC classification number: C07D307/12

    Abstract: The present invention relates to a process for the production of (−)3,4-divanillyl tetrahydrofiran of formula (2) which comprises (a) isolating) (−) secoisolariciresinol of formula (1) from the heartwood and roots of Taxus wallichiana by an improved process which consists of partitioning of the alcoholic extract of the heartwood and roots of T. wallichiana between water and chlorinated solvent, (b) extracting the chlorinated solvent extract with alkali and (c) isolating (−) secoisolariciresinol from the alkali extract upon neutralization with mineral acid and extracting with organic solvent and (d) crystallizing it from suitable organic solvent, (e) dissolving the isolated (−) secoisolariciresinol in suitable organic solvent and (f) reacting with triphenyl phosphine halide at 0-80° C. for 1-10 hours and (g) isolating (−) 3,4-divanillyl tetrahydrofuran by column chromatography.

    Abstract translation: 本发明涉及一种制备式(2)的( - )3,4-二氢化茚基四氢呋喃的方法,其包括(a)从红豆杉的心材和根中分离出( - )式(1)的( - )间二异硫氰菊酯 一种改进的方法,其包括在水和氯化溶剂之间分配心材的木材和根的酒精提取物,(b)用碱提取氯化溶剂提取物,和(c)从碱提取物中分离( - )二硫代亚铁氰菊酯, 用无机酸中和并用有机溶剂萃取,(d)从合适的有机溶剂中结晶,(e)将分离的( - )二异硫氰酸酯溶解在合适的有机溶剂中,和(f)在0-80℃与三苯基膦卤化物反应 (g)通过柱色谱法分离( - )3,4-二苯乙烯基四氢呋喃。

    Process for preparing novel biologically active synthetic molecule 4-(p-methoxyphenyl)-2-amino-butane
    6.
    发明授权
    Process for preparing novel biologically active synthetic molecule 4-(p-methoxyphenyl)-2-amino-butane 失效
    制备新型生物活性合成分子4-(对甲氧基苯基)-2-氨基 - 丁烷的方法

    公开(公告)号:US06252114B1

    公开(公告)日:2001-06-26

    申请号:US09535121

    申请日:2000-03-24

    CPC classification number: C07C43/225 C07C217/62

    Abstract: The invention provides a process for the preparation of 4-(p-methoxyphenyl)-2-aminobutane represented by structural formula (1) as shown herein below: [C11H17ON=4-(p-methoxy phenyl)-2-amino butane] said process comprising the steps of, (a) isolating a phenolic compound 4-hydroxyphenyl)-butan-2-ol from the leaves of Taxus wallichiana by known methods, (b) treating the phenolic compound in aqueous mineral acid to obtain a phenolic halide derivative, (c) converting the phenolic halide derivative into its methyl ether by treating it with a methating agent, (d) reacting the methyl ether halide with azide to obtain an azido derivative, and (e) hydrogenating the azido compound to obtain 4-(p-methoxyphenyl)-2-aminobutane.

    Abstract translation: 本发明提供了制备由结构式(1)表示的4-(对甲氧基苯基)-2-氨基丁烷的方法,如下所示:[C 11 H 17 ON = 4-(对甲氧基苯基)-2-氨基丁烷]所述 方法包括以下步骤:(a)通过已知方法从紫杉属的叶子中分离酚类化合物4-羟基苯基 - 丁-2-醇,(b)在无机酸水溶液中处理酚类化合物以获得酚卤化物衍生物 (c)通过用甲基化剂处理酚卤化物衍生物转化成甲基醚,(d)使甲基醚卤化物与叠氮化物反应得到叠氮基衍生物,和(e)氢化叠氮化合物得到4-( 对甲氧基苯基)-2-氨基丁烷。

    Process for the production of taxol
    7.
    发明授权
    Process for the production of taxol 失效
    紫杉醇生产工艺

    公开(公告)号:US5856532A

    公开(公告)日:1999-01-05

    申请号:US909810

    申请日:1997-08-12

    CPC classification number: C07D305/14

    Abstract: A process has been developed for production of taxols A, B, C with high yields from 7-xylosyl-10-deacetyl taxol A (taxol analogue A or, xyloside A), 7-xylosyl-10-deacetyl-taxol B (taxol analogue B or xyloside B), 7-xylosyl-10-deacetyl--taxol C (taxol analogue C or xyloside C), which comprises (i) isolating the taxol analogues A, B, C form the stembark of Taxus wallichiana by an improved process devoiding of solvent partitioning step, (ii) treating the isolated taxol analogues A, B, C with periodates in an acid free polar solvent medium to cleave the diol into dialdehyde at ambient temperature, (iii) reducing the dialdehyde solution with borohydride in a polar solvent--acetic acid medium at 0.degree.-40.degree. C. into an acetal, (iv) acidifying the resultant acetal with a mixture of mineral acid-polar solvent at 0.degree.-40.degree. C. into intermediate product 10-deacetyl taxols A, B, C, (V) reacting 10-deacetyl taxols A or B or C with a silane in presence of a base at 20.degree.-40.degree. C. to protect 2', 7-hydroxyl groups, of 10-deacetyl taxols A, B, C (vi) acetylating the 10-hydroxyl group in situ with an acetylating agent at 10.degree.-40.degree. C., (vii) deprotecting the 2', 7-hydroxyl groups with a mixture of mineral acid-polar solvent at 0.degree.-10.degree. C. (viii) isolating taxols A or B or C by chromatography over silica.

    Abstract translation: 已经开发了用于从7-木糖基-10-脱乙酰紫杉醇A(紫杉醇类似物A或木糖苷A),7-木糖基-10-脱乙酰基紫杉醇B(紫杉醇类似物)的高收率生产紫杉醇A,B,C的方法 B或木糖苷B),7-木糖基-10-脱乙酰基紫杉醇C(紫杉醇类似物C或木糖苷C),其包括(i)通过改进的方法脱除紫杉醇类似物A,B,C形成紫杉属 的溶剂分配步骤,(ii)在酸性极性溶剂介质中用高碘酸盐处理分离的紫杉酚类似物A,B,C,以在环境温度下将二醇切割成二醛,(iii)用极性溶剂中的硼氢化物还原二醛溶液 - 乙酸培养基在0°-40℃进入缩醛,(iv)在0-40℃下用无机酸 - 极性溶剂的混合物将所得缩醛酸化成中间产物10-脱乙酰基紫杉醇A,B C,(Ⅴ)在20℃-40℃下,使10-脱乙酰基的紫杉醇A或B或C与硅烷反应,保护2' ,10-脱乙酰基紫杉醇A,B,C(vi)的7-羟基,(vi)在10°-40℃用乙酰化剂原位乙酰化10-羟基,(vii)使2',7- 羟基与无机酸极性溶剂的混合物在0-10℃下进行。(viii)通过硅胶色谱分离紫杉醇A或B或C。

    Process for the production of 4-aryl-2 butanols from Taxus wallichiana
    10.
    发明授权
    Process for the production of 4-aryl-2 butanols from Taxus wallichiana 有权
    从Taxus wallichiana生产4-芳基-2丁醇的方法

    公开(公告)号:US06184367B2

    公开(公告)日:2001-02-06

    申请号:US09358113

    申请日:1999-07-21

    CPC classification number: C07H15/18 C07C37/004 C07H1/08 C07C39/11

    Abstract: The present invention provides a process for the production of two molecules of 4-aryl-2 butanols having the general formula 1 given below: Wherein R═H or glucose from the leaves of Taxus wallichiana, which comprises: (a) defatting air dried, pulverized leaves with aliphatic hydrocarbon solvents, (b) extracting the defatted leaves with chlorinated solvents and polar solvent successively at room temperature, (b) concentrating the chlorinated solvent soluble faction to a residue and treating the residue with aqueous solution of alkali and extracting with chlorinated solvents, (d) acidifying the alkali layer with mineral acid and extracting with ethyl acetate and concentrating the ethyl acetate phase to give compound of formula 1 where R═H, (e) concentrating the polar solvent fraction from step (b) to a residue and treating the residue with aqueous solution of alkali and extracting with chlorinated solvent, and (f) acidifying the alkali phase with mineral acid and extracting with ethyl acetate and concentrating the ethyl acetate to give compound of formula 1 where R=glucose.

    Abstract translation: 本发明提供了一种生产具有下列通式1的两分子的4-芳基-2丁醇的方法:其中R = H或来自红豆杉叶的葡萄糖,其包括:(a)将空气干燥脱脂, 用脂肪族烃溶剂粉碎叶片,(b)在室温下连续用氯化溶剂和极性溶剂萃取脱脂叶,(b)将氯化溶剂可溶部分浓缩至残留物,用碱水溶液处理残留物,用氯化物萃取 溶剂,(d)用无机酸酸化碱层并用乙酸乙酯萃取并浓缩乙酸乙酯相,得到其中R = H的式1化合物,(e)将步骤(b)的极性溶剂级分浓缩至残余物 并用碱水溶液处理残留物,用氯化溶剂萃取,(f)用无机酸酸化碱相,用乙酸乙酯萃取 并浓缩乙酸乙酯,得到其中R =葡萄糖的式1化合物。

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