Process for preparation of crystallized monohydrated sodium
phenylpyruvate
    1.
    发明授权
    Process for preparation of crystallized monohydrated sodium phenylpyruvate 失效
    结晶一水合苯丙酮酸钠的制备方法

    公开(公告)号:US4518800A

    公开(公告)日:1985-05-21

    申请号:US630427

    申请日:1984-07-13

    CPC分类号: C07C51/00 C07C51/41

    摘要: The invention concerns a process for preparation of crystallized monohydrated sodium phenylpyruvate comprising: hot reacting benzaldehyde in an aqueous medium in the presence of a catalytic quantity of ethanolamine with the stoichiometric quantity of hydantoin, then treating the reactional medium hot at pH=14 through an excess of sodium hydroxide, acidifying to pH=9 with concentrated hydrochloric acid the so obtained solution and separating the formed precipitate.

    摘要翻译: 本发明涉及一种制备结晶的一水合的苯基苯丙酮酸钠的方法,其包括:在催化量的乙醇胺与化学计量的乙内酰脲存在下,在含水介质中使苯甲醛热反应,然后在pH = 14的条件下将反应介质热处理过量 的氢氧化钠,用浓盐酸酸化至pH = 9,得到的溶液并分离形成的沉淀。

    Process for the preparation of crystalline sodium paraformylphenolate
    2.
    发明授权
    Process for the preparation of crystalline sodium paraformylphenolate 失效
    制备结晶多聚甲酚钠的方法

    公开(公告)号:US4346238A

    公开(公告)日:1982-08-24

    申请号:US147678

    申请日:1980-05-07

    CPC分类号: C07C47/565 C07C45/39

    摘要: Sodium paraformylphenolate crystallized with two molecules of water is manufactured by:(a) condensing glyoxylic acid with an excess of phenol in water in the presence of sodium hydroxide at a temperature comprised between 30.degree. C. and 100.degree. C.;(b) neutralizing the solution thus obtained and then freeing it from the unconverted phenol by steam distillation or extraction with a water-immiscible organic solvent and then subjecting it hot under a pressure of oxygen, to a catalytic decarboxylating oxidizing degradation in the presence of sodium hydroxide;(c) allowing the aqueous solution so-obtained, after removal of the catalyst by filtration, and then concentration hot under vacuum to 60% plus or minus 10% of its initial volume, to crystallize; and(d) draining the precipitated crystals, washing them and then drying them to constant weight under vacuum of 1 mm of mercury at 20.degree. C., to obtain sodium paraformylphenolate crystallized with 2 molecules of water or dried to constant weight under a vacuum of 1 mm of mercury at 100.degree. C. to obtain it in anhydrous form. The product is useful for preparing parahydroxy benzaldehyde quantitatively and without other purification reactions.

    摘要翻译: 用两分子水结晶的多聚甲硫醇钠是通过以下方法制造的:(a)在氢氧化钠存在下,在30℃至100℃的温度下,使乙醛酸与过量的苯酚在水中冷凝; (b)中和所得溶液,然后通过水蒸气蒸馏或与水不混溶的有机溶剂萃取,然后将其从未转化的苯酚中释出,然后在氧气压力下热处理,在钠存在下进行催化脱羧氧化降解 氢氧化物; (c)通过过滤除去催化剂后,使真空度为60%±10%,使其结晶,得到如此得到的水溶液。 和(d)排出沉淀的晶体,洗涤,然后在20℃下在1mm汞柱的真空下将其干燥至恒重,得到用2分子水结晶的多聚甲酰基苯酚钠,或在真空下干燥至恒重 在100℃下加入1毫米汞柱,以无水形式得到。 该产品可用于定量和无其他纯化反应制备对羟基苯甲醛。

    Process of preparation of racemic hydroxyarylglycolic acids and novel
products resulting therefrom
    3.
    发明授权
    Process of preparation of racemic hydroxyarylglycolic acids and novel products resulting therefrom 失效
    制备外消旋羟基芳基乙醇酸及其产生的新产品的方法

    公开(公告)号:US4339602A

    公开(公告)日:1982-07-13

    申请号:US243965

    申请日:1981-02-25

    CPC分类号: C07C51/367

    摘要: The invention relates to a process of preparation of racemic hydroxyarylglycolic acids and the novel products resulting therefrom.According to such process glyoxylic acid is condensed in water in the presence of an alkaline agent at a temperature of between 35.degree. and 100.degree. C., on an excess, or not, of phenolic aromative derivative other than phenol, having at least one proton on either of the ortho or para positions with respect to the phenol function.Application to the production of novel acids such as 4-hydroxy 3-tertiobutyl mandelic acid, 2-hydroxy 5-tertiobutyl mandelic acid, 3-chloro 4-hydroxy mandelic acid, 2-fluoro 4-hydroxy mandelic acid, monohydrated 3,5-dimethoxy 4-hydroxy mandelic acid, 2-hydroxy 5-methyl mandelic acid, (1-hydroxy 2-naphthyl) glycolic acid, 4-ethyl 2-hydroxy mandelic acid, and 4-hydroxy 3-methyl mandelic acid.

    摘要翻译: PCT No.PCT / FR80 / 00126 Sec。 371日期:1981年2月25日 102(e)日期1981年2月25日PCT提交1980年7月24日PCT公布。 公开号WO81 / 00254 日本2月5日,1981年。本发明涉及外消旋羟基芳基乙醇酸的制备方法和由此产生的新产物。 根据这种方法,乙醛酸在碱性试剂存在下,在35℃至100℃的温度下,在除苯酚以外的酚类芳族衍生物的过量或不存在下,在水中冷凝,其具有至少一个质子 在相对于酚官能团的邻位或对位。 适用于生产新型酸如4-羟基-3-叔丁基扁桃酸,2-羟基5-叔丁基扁桃酸,3-氯-4-羟基扁桃酸,2-氟4-羟基扁桃酸,一水合3,5-二 二羟甲基4-羟基扁桃酸,2-羟基-5-甲基扁桃酸,(1-羟基2-萘基)乙醇酸,4-乙基2-羟基扁桃酸和4-羟基3-甲基扁桃酸。

    Process for manufacturing N-acyl derivatives of glycines
.alpha.-substituted by radicals of aromatic nature and novel products
thereof
    4.
    发明授权
    Process for manufacturing N-acyl derivatives of glycines .alpha.-substituted by radicals of aromatic nature and novel products thereof 失效
    用于制备由芳香族自由基取代的甘氨酸N-酰基衍生物的方法及其新产物

    公开(公告)号:US4088657A

    公开(公告)日:1978-05-09

    申请号:US722286

    申请日:1976-09-10

    CPC分类号: C07C233/45

    摘要: This is an improved process of manufacturing N-acyl derivatives of glycines .alpha.-substituted by radicals with an aromatic nature by condensation of the addition product of glyoxylic acid and an amide, with an aromatic compound. In a first stage, the reaction is carried out at low temperature, in a concentrated sulfuric medium, of an aliphatic nitrile of the formula R--C.tbd.N in which R is a radical selected from the group of substituted and unsubstituted, saturated and unsaturated alkyl radicals, with a concentrated aqueous solution of glyoxylic acid. Then in a second stage, the mixture obtained is condensed also at low temperature with a compound of aromatic nature not including a hydroxyl group and having at least one substitutable free hydrogen, and the resulting product is collected. The concentrated sulfuric acid may be supplemented with acetic acid during the second stage. A surface active agent may be also added in this stage. The products are valuable intermediates for the preparation of semi-synthetic penicillins.

    摘要翻译: 这是通过将乙醛酸和酰胺的加成产物与芳族化合物缩合制备具有芳香性的基团被α-取代的甘氨酸的N-酰基衍生物的改进方法。 在第一阶段中,反应在低浓度的硫酸介质中进行,其中R为选自取代和未取代的饱和和不饱和烷基的基团的式RC 3BOND N的脂族腈 ,用浓缩的乙醛酸水溶液。 然后在第二阶段中,所获得的混合物也在低温下与芳族性质不包含羟基并具有至少一个可取代的游离氢的化合物一起冷凝,并收集所得产物。 浓硫酸在第二阶段可补充乙酸。 在该阶段也可以加入表面活性剂。 该产品是制备半合成青霉素的有价值的中间体。

    Method of preparation of 6-aza uracile and its O-disilyl derivative
    5.
    发明授权
    Method of preparation of 6-aza uracile and its O-disilyl derivative 失效
    6-氮杂尿嘧啶及其O-二甲硅烷基衍生物的制备方法

    公开(公告)号:US3983114A

    公开(公告)日:1976-09-28

    申请号:US625839

    申请日:1975-10-24

    IPC分类号: C07D253/06 C07F7/18

    CPC分类号: C07F7/1856 C07D253/06

    摘要: A method of preparation of 6-aza uracile, comprising the steps of:A. Cyclization of semi-carbazone of glyoxylic acid by heating this latter with an excess of a trialkyl-silylation agent taken as a solvent and isolating the resulting product, namely the O-disilylated derivative of 6-aza uracile (or di-3,5 (trialkylsiloxy)1,2,4 triazine) andB. subjection of the product resulting from step a) to an acid hydrolysis.

    摘要翻译: 一种制备6-氮杂尿嘧啶的方法,包括以下步骤:

    Acetaldehyde derivatives, their preparation process and their use
    7.
    发明授权
    Acetaldehyde derivatives, their preparation process and their use 失效
    乙醛衍生物,其制备方法及其用途

    公开(公告)号:US5527964A

    公开(公告)日:1996-06-18

    申请号:US431033

    申请日:1995-04-28

    摘要: Azines of formula (I): ##STR1## in which R and R' either are identical and represent an alkyl radical containing 1 to 4 carbon atoms or an alkenyl radical containing 3 to 5 carbon atoms, or together form a radical of formula (II):--CHR.sub.1 --(CR.sub.2 R.sub.3).sub.n --CHR.sub.4 -- (II)in which R.sub.1, R.sub.2, R.sub.3 and R.sub.4, identical or different, represent a hydrogen atom or an alkyl radical containing 1 to 4 carbon atoms and n represents 0 or 1, in their different stereoisomer forms, their preparation process and their use.

    摘要翻译: 式(I)的吖嗪:其中R和R'相同并且表示含有1至4个碳原子的烷基或含有3至5个碳原子的烯基,或一起形成基团 式(II):-CHR1-(CR2R3)n-CHR4-(Ⅱ),其中R1,R2,R3和R4相同或不同,表示氢原子或含有1至4个碳原子的烷基,n表示0 或1,以其不同的立体异构体形式,其制备方法及其用途。

    Preparation process for hydroxyphenylacetic acids
    8.
    发明授权
    Preparation process for hydroxyphenylacetic acids 失效
    羟基苯乙酸的制备方法

    公开(公告)号:US5395964A

    公开(公告)日:1995-03-07

    申请号:US245898

    申请日:1994-05-19

    CPC分类号: C07C51/377

    摘要: Preparation process for a hydroxyphenylacetic acid of formula (I): ##STR1## where R.dbd.H, alkyl or alkoxyl as well as its salts, in which the corresponding free or salified hydroxymandelic acid of formula (II): ##STR2## in which R has the meaning given previously and M.dbd.H, K or an ammonium group is reacted in an aqueous medium, at a temperature greater than or equal to 50.degree. C., with formic acid in the presence of catalytic quantities of an oxygenated derivative of sulphur having a degree of oxidation from 2 to 4, in order to obtain the hydroxyphenylacetic acid of formula (I) which is isolated or, if desired, is salified according to the usual methods and the hydroxyphenylacetic acid thus obtained.

    摘要翻译: 式(I)的羟基苯基乙酸的制备方法:其中R = H,烷基或烷氧基及其盐,其中相应的式(II)的游离或盐化的羟基扁桃酸: (II)其中R具有先前给出的含义,M = H,K或铵基在水性介质中,在大于或等于50℃的温度下,与甲酸在催化量存在下反应 的氧化度为2至4的硫的氧化衍生物,以获得分离的或如果需要,根据常规方法成盐的式(I)的羟基苯基乙酸和由此获得的羟基苯基乙酸。

    Process for industrial manufacture of sodium parahydroxymandelate
    9.
    发明授权
    Process for industrial manufacture of sodium parahydroxymandelate 失效
    工业制造对羟基扁桃酸钠的方法

    公开(公告)号:US4978784A

    公开(公告)日:1990-12-18

    申请号:US426352

    申请日:1989-10-25

    申请人: Yani Christidis

    发明人: Yani Christidis

    CPC分类号: C07C51/367 C07C51/412

    摘要: This process is characterized by the fact that glyoxylic acid in aqueous solution is reacted with an excess of phenol in the presence of a tertiary amine, insoluble or slightly soluble in water and liquid at ambient temperature, in particular tributylamine or triisooctylamine, then the parahydroxymandelic acid thus obtained is salified with sodium hydroxide in aqueous solution.The reaction of the glyoxylic acid with phenol is carried out at a temperature between 15.degree. C. and 80.degree. C.

    摘要翻译: 该方法的特征在于水溶液中的乙醛酸与过量的苯酚在叔胺的存在下反应,在环境温度下不溶或微溶于水和液体,特别是三丁胺或三异辛胺,然后将对羟基扁桃酸 得到的溶液用氢氧化钠在水溶液中成盐。 乙醛酸与苯酚的反应在15℃至80℃的温度下进行。

    Process to manufacture glyoxylic acid by electrochemical reduction of
oxalic acid
    10.
    发明授权
    Process to manufacture glyoxylic acid by electrochemical reduction of oxalic acid 失效
    通过电化学还原草酸制备乙醛酸的方法

    公开(公告)号:US4692226A

    公开(公告)日:1987-09-08

    申请号:US901792

    申请日:1986-08-29

    IPC分类号: C25B3/04 C07B29/06 C07C51/40

    CPC分类号: C25B3/04

    摘要: This process, carried out at a temperature of 0.degree. to 30.degree. C. in an electrolyzer outfit consisting of at least one anode compartment containing an anode and anolyte, comprising an aqueous acid solution, at least one cathode compartment containing a cathode and catholyte, comprising an aqueous solution of oxalic acid and, between the two compartments, at least one separator, is characterized by the fact that the anode is made of a solid conductor uniformly coated with lead dioxide.

    摘要翻译: 该方法在由包含阳极和阳极电解液的至少一个阳极室组成的电解装置中在0℃至30℃的温度下进行,包含酸水溶液,至少一个含有阴极和阴极电解液的阴极室, 包括草酸水溶液,并且在两个室之间,至少一个分离器的特征在于阳极由均匀涂覆有二氧化铅的固体导体制成。