专利号:US-10294196-B2 优先权日:2015-11-18 标题:Process for the synthesis of intermediates useful for preparing 1,3,4-triazine derivatives 发明人:XU SHENG; XU YIHUI 权利人:FMC CORP 摘要:A process for the synthesis of 1,3-diethyl 2-(2-methylhydrazinylidene)propanedioate comprising the step of: reacting 2-halosubstituted diethyl malonate or mixtures of 2-halo-substituted diethyl malonates with methylhydrazine or the salt thereof in the presence of an acid catalyst is disclosed. 1,3-diethyl 2-(2-methylhydrazinylidene)propanedioate is an intermediate useful for preparing 1,3,4-triazines.
专利号:US-6538153-B1 优先权日:2001-09-25 标 题:Method of synthesis of water soluble fullerene polyacids using a macrocyclic malonate reactant 发明人:HIRSCH ANDREAS; REUTHER UWE 权利人:SIXTY INC C 摘要:A method for synthesizing compounds of the formulawhere C60 is a C60 fullerene. The method comprises the steps of forming a macrocyclic malonate compound of the formulawhere each Z is the same or different and is a straight-chain or branched-chain aliphatic radical having from 1-30 carbon atoms which may be unsubstituted or monosubstituted or polysubstituted by identical or different substitutents, in which radicals up to every third CH2 unit can be replaced by O or NR where R is alkyl having 1-20 carbon atoms or a chain containing unsubstituted or substituted aryl or other cyclic groups and n is an integer from 2 to 10; reacting said macrocyclic malonate compound with C60 to form an adduct of the formulawhere the Z radicals are linked together to form said macrocycle adduct; and hydrolyzing said macrocycle adduct to form a compound of the formula
专利号:US-2006047167-A1 优先权日:2004-09-02 标题 :Method of synthesis of water soluble fullerene polyacids using a malonate reactant 发明人:HIRSCH ANDREAS; BEUERLE FLORIAN; CHRONAKIS NIKOS 权利人:HIRSCH ANDREAS; BEUERLE FLORIAN; CHRONAKIS NIKOS 摘要:In one embodiment, the present invention is directed to a method for synthesizing compounds of the formula n n nwhere C m is a fullerene having m carbon atoms, the method comprising the steps of forming a linear malonate compound of the formula n n nwhere each Z is the same or different and is a straight-chain or branched-chain aliphatic radical having from 1-30 carbon atoms which may be unsubstituted or monosubstituted or polysubstituted by identical or different substitutents, in which radicals up to every third —CH 2 — unit can be replaced by O or NR″, n is an integer from 2 to 10, and the unfilled valences of the first and nth malonate groups are filled with bonds to hydrogen, a hydrocarbon group or substituted hydrocarbon group having 1-20 carbon atoms, or a chain containing unsubstituted or substituted aryl or other cyclic groups; or (ii) a branched malonate compound of the formula n n nwhere Z′ is an aliphatic radical having from 1-30 carbon atoms which may be unsubstituted or monosubstituted or polysubstituted by identical or different substitutents, in which radicals up to every third —CH 2 — unit can be replaced by O or NR″; and n is an integer from 2 to 10; n n reacting said malonate compound with C m to form an adduct of the formula n neach Z is bonded to both one carboxylate group of a first malonate moiety and one carboxylate group of a second malonate moiety and the unfilled valences of the first and nth malonate groups are filled with bonds to hydrogen, a hydrocarbon group or substituted hydrocarbon group having 1-20 carbon atoms, or a chain containing unsubstituted or substituted aryl or other cyclic groups; and hydrolyzing said adduct to form the compound.
专利号:WO-2006028776-A1 优先权日:2004-09-02 标题:Method of synthesis of water soluble fullerene polyacids using a malonate reactant 发明人:HIRSCH ANDREAS 权利人:SIXTY INC C; HIRSCH ANDREAS 摘要:A method for synthesizing compounds of the formula (I) where Cm is a fullerene having m carbon atoms and each R is independently -H or -Râ€? COOH where R is alkyl having 1-20 carbon atoms, substituted alkyl having 1-20 carbon atoms, alkenyl having 1-20 carbon atoms, substituted alkenyl having 1-20 carbon atoms, or a chain containing unsubstituted or substituted aryl or other cyclic groups, the method comprising the steps of forming a linear or branched malonate compound and hydrolyzing said adduct to form the compound.
专利号:US-4503252-A 优先权日:1979-09-10 标题:Process for the preparation of serinol and of serinol derivatives, and products obtained therefrom 发明人:FELDER ERNST; BIANCHI SERGIO; BOLLINGER HEINRICH 权利人:EPROVA AG 摘要:A method for the synthesis of serinol and serinol derivatives substituted at the nitrogen atoms by reacting a lower 1,3-dialkoxy-isopropyl halide with ammonia or an amine to form a 1,3-dialkoxy-isopropylamine and then removing the ether groups by heating with a hydrogen halide acid. The method allows the production of serinol and serinol derivatives using inexpensive starting materials in a simple manner and obtaining a high purity product which is free of interfering isomers. Novel compounds obtained by the method which are useful as pharmaceutical intermediates, X-ray contrasting agents and cytostatic or psychopharmacological drugs are also disclosed.
专利号:US-6448412-B1 优先权日:1995-07-31 标题:Methods for the preparation and characterization of multi-substituted fullerenes 发明人:MURPHY RANDALL B; WILSON STEPHEN R; LU QUING 权利人:SPHERE BIOSYSTEMS INC 摘要:The invention is directed to multiply-substituted fullerene derivatives of novel configurations, and methods for their preparation and use. The methods involve the combinatorial synthesis of a library of fullerene derivatives and comprises the steps of forming a mixture of fullerene derivatives by reacting the C n fullerene with two or more reactive precursor compounds, and removing the unreacted compounds to yield the fullerene derivatives having the desired activity. Methods for the identification and screening of a combinatorial library of fullerenes by 3 He-nuclear magnetic resonance and electrospray mass spectrometry to define members with the optimal desired activity are also provided.
[参考文献]: Shefang Ye, Et Al. Carboxylic Acid Fullerene (C60) Derivatives Attenuated Neuroinflammatory Responses By Modulating Mitochondrial Dynamics. Nanoscale Res Lett. 2015 Dec;10(1):953.
合成参考文献
摘要:Stará, I. G.; Starý, I., Science of Synthesis, (2010) 45, 1129. 摘要:Landais, Y., Science of Synthesis Knowledge Updates, (2013) 3, 61. 摘要:Araki, S.; Hirashita, T., Science of Synthesis Knowledge Updates, (2010) 4, 148. 摘要:Kwiecień, H., Science of Synthesis Knowledge Updates, (2014) 4, 103. 摘要:Cheng, B.; Wang, T., Science of Synthesis Knowledge Updates, (2020) 3, 220.