Methods for preparing amides and amino acids
    1.
    发明授权
    Methods for preparing amides and amino acids 有权
    制备酰胺和氨基酸的方法

    公开(公告)号:US08637696B2

    公开(公告)日:2014-01-28

    申请号:US13621553

    申请日:2012-09-17

    摘要: The invention provides novel compounds and methods to carry out organocatalytic Michael additions of aldehydes to nitroethylene catalyzed by a proline derivative to provide α-substituted-γ-nitroaldehydes. The reaction can be rendered enantioselective when a chiral pyrrolidine catalyst is used, allowing for Michael adducts in nearly optically pure form (e.g., 96-99% e.e.). The Michael adducts can bear a single substituent or dual substituents adjacent to the carbonyl. The Michael adducts can be efficiently converted to protected γ2-amino acids, which are essential for systematic conformational studies of γ-peptide foldamers.

    摘要翻译: 本发明提供了新的化合物和方法,用于通过脯氨酸衍生物进行有机催化迈克尔加成醛到硝基亚乙基以提供α-取代的γ-硝基醛。 当使用手性吡咯烷催化剂时,反应可以呈现为对映选择性,允许以几乎光学纯的形式(例如96-99%e.e。)的迈克尔加合物。 迈克尔加合物可以承受单个取代基或与羰基相邻的双取代基。 迈克尔加合物可以有效地转化为受保护的γ2-氨基酸,这对于γ-肽折叠物的系统构象研究至关重要。

    Preparation of N-alkenyl carboxamides
    3.
    发明授权
    Preparation of N-alkenyl carboxamides 失效
    N-烯基甲酰胺的制备

    公开(公告)号:US5710331A

    公开(公告)日:1998-01-20

    申请号:US548724

    申请日:1995-10-26

    CPC分类号: C07C231/08

    摘要: Preparation of N-alkenyl carboxamides of the general formula I ##STR1## in which the radicals R.sup.1 to R.sup.4 independently stand for hydrogen or for aliphatic, cycloaliphatic, or aromatic radicals, which optionally carry inert substituents, wherein an amide of the general formula II ##STR2## in which the radical R.sup.1 has the above meaning, and a carbonyl compound of the general formula III ##STR3## in which the radicals R.sup.2 to R.sup.4 have the above meanings, are caused to react in the presence of a base, said reaction being either a) carried out in the presence of a carboxylic acid derivative of the general formula IV ##STR4## in which the radical R.sup.5 stands for hydrogen or an alkyl or aryl group and X is a halogen, alkoxy, or carboxylalkyl radical, or b) continued in the presence of a carboxylic acid derivative of the formula IV, and the amide of the formula I is isolated.

    摘要翻译: 其中基团R 1至R 4独立地代表氢或用于任选地带有惰性取代基的脂族,脂环族或芳族基团的通式I(I)的N-烯基甲酰胺的制备,其中一般的酰胺 其中基团R 1具有上述含义的式II(II)和其中基团R 2至R 4具有上述含义的通式III(III)的羰基化合物进行反应 碱的存在,所述反应是a)在通式IV(IV)的羧酸衍生物存在下进行,其中基团R 5代表氢或烷基或芳基,X是 卤素,烷氧基或羧基烷基,或b)在式Ⅳ的羧酸衍生物存在下连续进行,分离式Ⅰ的酰胺。

    Preparation of aqueous solutions of acetoacetamide
    4.
    发明授权
    Preparation of aqueous solutions of acetoacetamide 失效
    乙酰乙酰胺水溶液的制备

    公开(公告)号:US5025106A

    公开(公告)日:1991-06-18

    申请号:US600648

    申请日:1990-10-22

    申请人: Steven L. Cook

    发明人: Steven L. Cook

    CPC分类号: C07C231/04

    摘要: Disclosed is a process for the preparation of aqueous solutions of acetoacetamide wherein diketene and aqueous ammonia having an ammonia concentration of about 6.0 to 9.0 weight percent are continuously fed to a reaction zone at rates which maintain in the reaction zone a pH of about 7.0 to 8.2 and a residence time of about 20 to 150 minutes while (i) maintaining the temperature of the reaction zone at about 40.degree. to 75.degree. C. and (ii) subjecting the contents of the reaction zone to vigorous agitation. An aqueous product solution having an acetoacetamide concentration of about 25 to 35 weight percent is continuously removed from the reaction zone.

    摘要翻译: 公开了一种制备乙酰乙酰胺水溶液的方法,其中具有约6.0至9.0重量%的氨浓度的二烯酮和氨水以维持反应区pH为约7.0至8.2的速率连续进料至反应区 停留时间为约20至150分钟,同时(i)将反应区的温度保持在约40℃至75℃,和(ii)使反应区的内容物剧烈搅拌。 乙酰乙酰胺浓度约为25〜35重量%的水溶液从反应区连续除去。

    Preparation of acetoacetarylamides
    6.
    发明授权
    Preparation of acetoacetarylamides 失效
    乙酰乙酰胺的制备

    公开(公告)号:US5523486A

    公开(公告)日:1996-06-04

    申请号:US326100

    申请日:1994-10-19

    IPC分类号: C07C231/04 C07C235/80

    CPC分类号: C07C231/04

    摘要: A process for preparing acetoacetarylamides of the formula I ##STR1## where R.sup.1 and R.sup.2 are identical or different alkyl radicals,l and m are each 0, 1 or 2, andis 0 or 1,by addition of diketene to the appropriate arylamine by continuously reacting the arylamine with diketene in the presence of a mixture of water and of a (C.sub.1 -C.sub.4)-alkanol at temperatures from 60.degree. C. to 100.degree. C. in the course of from 0.1 to 10 min.

    摘要翻译: 制备式I的乙酰乙酰胺的方法,其中R 1和R 2是相同或不同的烷基,l和m各自为0,1或2,并且为0或1,通过连续地向适当的芳基胺中加入双烯酮 在0.1至10分钟的过程中,在水和(C 1 -C 4) - 烷醇的混合物存在下,使芳基胺与双烯酮反应,其温度为60℃至100℃。

    Process for the manufacture of .beta.-isobutyrylaminocrotonic acid amide
    10.
    发明授权
    Process for the manufacture of .beta.-isobutyrylaminocrotonic acid amide 失效
    制备β-异丁酰氨基巴豆酸酰胺的方法

    公开(公告)号:US4242276A

    公开(公告)日:1980-12-30

    申请号:US99778

    申请日:1979-12-03

    申请人: Bernd Schilling

    发明人: Bernd Schilling

    CPC分类号: C07C231/00

    摘要: A process for the manufacture of .beta.-isobutyrylaminocrotonic acid amide by reacting .beta.-aminocrotonic acid amide with dimethylketene in the liquid or gaseous state without the application of external heat at temperatures in the range of from room temperature to 70.degree. C. The dispersion medium used is an organic solvent having a boiling point above 40.degree. C. that may contain up to 0.1 mole of water and 0.2 to 2 moles of a carboxylic acid having 1 to 4 carbon atoms per mole of .beta.-aminocrotonic acid amide. If the dimethylketene is added undiluted the reaction is carried out in the absence of oxygen and in the presence of a protective gas atmosphere. The .beta.-isobutyrylaminocrotonic acid amide is obtained in the form of two stereoisomers (Z- and E-forms), which differ as regards their melting point and their solubility in organic solvents. On heating to 40.degree. C., the E-form is converted into the Z-form.

    摘要翻译: 通过使β-氨基巴豆酸酰胺与液体或气态的二甲基烯酮反应制备β-异丁酰氨基巴豆酸酰胺的方法,而不需要在室温至70℃的温度范围内施加外界热。使用的分散介质 是沸点高于40℃的有机溶剂,其可含有至多0.1摩尔水和0.2至2摩尔每摩尔β-氨基巴豆酸酰胺具有1至4个碳原子的羧酸。 如果未稀释地加入二甲基烯酮,则反应在不存在氧的情况下和在保护气体气氛存在下进行。 β-二异丁酰氨基巴豆酸酰胺以两种立体异构体(Z-和E-型)的形式获得,它们的熔点和它们在有机溶剂中的溶解度不同。 加热至40℃时,将E型转化成Z型。