Preparation of riboflavin, and
4,5-dimethyl-N-(D)-ribityl-2-(O-alkoxyphenylazo)-aniline intermediates
    1.
    发明授权
    Preparation of riboflavin, and 4,5-dimethyl-N-(D)-ribityl-2-(O-alkoxyphenylazo)-aniline intermediates 失效
    制备核黄素和4,5-二甲基-N-(D) - 二丙基-2-(O-烷氧基苯偶氮) - 苯胺中间体

    公开(公告)号:US4656275A

    公开(公告)日:1987-04-07

    申请号:US730056

    申请日:1985-05-03

    CPC分类号: C07D475/14

    摘要: An improved process for the preparation of riboflavin by condensation of a 4,5-dimethyl-N-(D)-ribityl-2-phenylazoaniline derivative with barbituric acid in the presence of an acidic condensing agent in an organic solvent, wherein a 4,5-dimethyl-N-(D)-ribityl-2-(o-alkoxyphenylazo)-aniline of the formula IIa ##STR1## where R is alkyl of 1 to 4 carbon atoms, in particular methyl, is reacted with barbituric acid, as well as the novel intermediates of the formula IIa.

    摘要翻译: 一种改进的制备核黄素的方法,其通过在酸性缩合剂存在下,在有机溶剂中使4,5-二甲基-N-(D) - 间苯基] -2-苯基偶氮苯胺衍生物与巴比妥酸缩合, 其中R是1至4个碳原子的烷基,特别是甲基的式IIa的(R) - (2-(O-)烷基-2-(邻 - 烷氧基苯基偶氮) - 苯胺其中R是与巴比妥酸反应, 以及式IIa的新型中间体。

    Preparation of canthaxanthin and astaxanthin
    5.
    发明授权
    Preparation of canthaxanthin and astaxanthin 失效
    甘氨酸和阿司匹林的制备

    公开(公告)号:US5210314A

    公开(公告)日:1993-05-11

    申请号:US695336

    申请日:1991-04-29

    摘要: A process for preparing canthaxanthin (Ia) and astaxanthin (Ib) of the formula I ##STR1##where R is H (a) or OH (b), comprises reacting a tertiary alcohol of the formula II ##STR2##where R is H (a) or OH (b), with trifluoroacetic acid, reacting the resulting novel trifluoroacetate of the formula III ##STR3##with triphenylphosphine, and reacting the resulting novel triphenylphosphonium trifluoroacetate of the formula IV ##STR4## with 2,7-dimethyl-2,4,6-octatriene-1,8-dial under the conditions of a Wittig synthesis. The present invention also relates to the novel trifluoroacetates of the formula III and the corresponding triphenylphosphonium trifluoroacetates of the formula IV.

    摘要翻译: 制备式I的角黄素(Ia)和虾青素(Ib)的方法,其中R是H(a)或OH(b))包括使式II的叔醇(II)与R (III)的三氟乙酸盐与三苯基膦反应,并使得到的式IV的三氟化三苯基鏻(Ⅳ)与式(Ⅳ)化合物反应,得到新的三氟乙酸盐, 在Wittig合成条件下用2,7-二甲基-2,4,6-辛二烯-1,8-表盘。 本发明还涉及式III的新型三氟乙酸盐和式Ⅳ相应的三苯基三氟乙酸盐。

    Preparation of 2-n-propyl-4-amino-5-methoxymethyl-pyrimidine
    6.
    发明授权
    Preparation of 2-n-propyl-4-amino-5-methoxymethyl-pyrimidine 失效
    2-正丙基-4-氨基-5-甲氧基甲基 - 嘧啶的制备

    公开(公告)号:US4918191A

    公开(公告)日:1990-04-17

    申请号:US393976

    申请日:1989-08-15

    IPC分类号: C07D239/42

    CPC分类号: C07D239/42

    摘要: In an improved process for the preparation of 2-n-propyl-4-amino-5-methoxymethyl-pyrimidine of the formula I ##STR1## by reacting butyramidine II ##STR2## with .alpha.-methoxymethyl-.beta.-methoxyacrylonitrile III ##STR3## the butyramidine II is reacted with a 0.4-5 molar excess of .alpha.-methoxymethyl-.beta.-methoxyacrylonitrile III at from -10.degree. to +20.degree. C.

    摘要翻译: 通过使丁酰脒II II与α​​-甲氧基甲基-β-甲氧基丙烯腈III反应制备式I的2-正丙基-4-氨基-5-甲氧基甲基 - 嘧啶的改进方法III IMA图 > III,在-10℃至+ 20℃下,使丁酰脒II与0.4-5摩尔过量的α-甲氧基甲基-β-甲氧基丙烯腈III反应。

    Epimerization of sugars, in particular of D-arabinose to D-ribose
    7.
    发明授权
    Epimerization of sugars, in particular of D-arabinose to D-ribose 失效
    糖异构化,特别是D-阿拉伯糖对D-核糖

    公开(公告)号:US4778531A

    公开(公告)日:1988-10-18

    申请号:US68171

    申请日:1987-06-30

    CPC分类号: C07H3/02

    摘要: Pentoses and hexoses are epimerized by heating sugar dissolved in a solvent in the presence of a molybdenum(VI) compound, by an improved process in which, for the preparation of a sugar having cis OH groups in the 2- or 3-position, of the formula Ia or Ib ##STR1## where R is one of the radicals ##STR2## a homogeneous solution of the corresponding sugar of the formula IIa or IIb ##STR3## is heated to 75.degree.-100.degree. C. in the presence of from 30 to 200 mol %, based on sugar used, of a metal salt of the formula (III)MeX.sub.2 (III)where Me is Mg, Ca, Sr, Ba or Zn and X is Cl or Br, which may or may not contain water of crystallization, and in the presence of from 2 to 20 mol %, based on the sugar used, of a molybdenum(VI) compound.The process is particularly important for the preparation of D-ribose, which is required as an intermediate for vitamin B.sub.2.

    摘要翻译: 戊糖和己糖通过加热溶解在钼(VI)化合物存在下的溶剂中的糖进行差向异构化,其中通过改进方法,其中为了制备在2-或3-位具有顺式OH基团的糖, 式Ia或Ib的化合物,其中R是式IIa或IIb的相应糖的均匀溶液之一的基团之一,在30℃的存在下加热至75℃-100℃ (III)的MeX2(III)的金属盐,其中Me是Mg,Ca,Sr,Ba或Zn,X是Cl或Br,其可以含有或可以不含水 的结晶,并且在基于所用糖的2至20摩尔%的存在下,使用钼(VI)化合物。 该方法对于制备作为维生素B2的中间体的D-核糖是特别重要的。

    Preparation of .alpha.-tocopherol
    8.
    发明授权
    Preparation of .alpha.-tocopherol 失效
    α-生育酚的制备

    公开(公告)号:US4550182A

    公开(公告)日:1985-10-29

    申请号:US588374

    申请日:1984-03-12

    CPC分类号: C07D311/72

    摘要: A process for the preparation of .alpha.-tocopherol of the formula I ##STR1## by reacting a chroman derivative with a C.sub.14 -Grignard reagent using a di-alkali metal tetrahalocuprate catalyst in a Schlosser-Fouquet reaction, wherein a chroman derivative of the general formula II ##STR2## where Y is a leaving group, especially Br, is used and is reacted, at from -70.degree. to 0.degree. C., first with a solution of about 1 equivalent of a Grignard compound of the general formula IIIX--Mg--R (III)where X is Cl, Br or I and R is straight-chain or branched alkyl of 1 to 14 carbon atoms, preferably methyl, ethyl or ##STR3## and then with a solution of a Grignard reagent of the formula IIIa ##STR4## in an ether solvent and a solution of a di-alkali metal tetrahalocuprate in an ether solvent. The novel process simplifies the preparation of 2RS,4'RS,8'RS-, 2R,4'RS,8'RS- or 2R,4'R,8'R-.alpha.-tocopherol by reacting a chroman structural unit, containing a C.sub.2 side-chain in the 2-position, with the corresponding C.sub.14 -Grignard compound.

    摘要翻译: 通过在Schlosser-Fouquet反应中使用二碱金属四卤代硼酸催化剂使苯并二氢吡喃衍生物与C14-格氏试剂反应制备式I的α-生育酚的方法,其中将 使用其中Y为离去基团,特别是Br的通式II(II),并且在-70℃至0℃下反应,首先用约1当量的Grignard化合物 通式III X-Mg-R(III)其中X为Cl,Br或I,R为1至14个碳原子的直链或支链烷基,优选为甲基,乙基或者“ 式IIIa的格利雅试剂(IIIa)在醚溶剂中和二碱金属四卤代硼酸酯在醚溶剂中的溶液。 该新方法简化了2RS,4'RS,8'RS-,2R,4'RS,8'RS-或2R,4'R,8'R-α-生育酚的制备,通过使色结构单元反应, 2-位的C2侧链与相应的C14-格利雅化合物。

    Preparation of riboflavin
    9.
    发明授权
    Preparation of riboflavin 失效
    核黄素的制备

    公开(公告)号:US4567261A

    公开(公告)日:1986-01-28

    申请号:US570457

    申请日:1984-01-13

    IPC分类号: C07D475/14 C07D475/02

    CPC分类号: C07D475/02

    摘要: Riboflavin of the formula I ##STR1## is prepared by condensing a 4,5-dimethyl-N-(D)-ribityl-2-phenylazoaniline of the formula II ##STR2## where R is H or --Cl, --NO.sub.2 or --CH.sub.3 in the o- or p-position, with barbituric acid of the formula III ##STR3## in the presence of an acid as the condensing agent, by an improved process in which the acidic condensing agent used is an aliphatic or cycloaliphatic/aliphatic tertiary carboxylic acid of the general formula IV ##STR4## where R.sup.1, R.sup.2 and R.sup.3 are each a lower alkyl group, R.sup.1, R.sup.2 and R.sup.3 together containing 3 to 20, preferably 3 to 10, carbon atoms, or R.sup.1 is a lower alkyl group, in particular methyl, and R.sup.2 and R.sup.3 together form a tetramethylene or pentamethylene group.The process can be particularly advantageously carried out using trimethylacetic acid or a commercial mixture of saturated tertiary carboxylic acids, e.g. Versatic .sup.R 10-acid.

    摘要翻译: 式I(I)的核黄素通过将式II的4,5-二甲基-N-(D) - 二乙基苯基偶氮苯胺(II)缩合制备,其中R是H或-Cl ,在邻位或对位的-NO 2或-CH 3与通式III的巴比妥酸(III)在作为缩合剂的酸存在下,通过改进的方法,其中使用酸性缩合剂 是通式IV(IV)的脂族或脂环族/脂肪族三羧酸,其中R 1,R 2和R 3各自为低级烷基,R 1,R 2和R 3一起含有3至20,优选3至10, 碳原子,或R 1是低级烷基,特别是甲基,R 2和R 3一起形成四亚甲基或五亚甲基。 该方法可以特别有利地使用三甲基乙酸或饱和叔羧酸的商业混合物,例如, 通用R10酸。