bis(diethylammonium) oxalate

• 分子结构分类: 有机化合物 - 有机酸及其衍生物 - 羧酸及其衍生物
• 英文名称: bis(diethylammonium) oxalate
• 英文别名: diethyl ammonium oxalate；Diethylammonium hydrogen oxalate；diethylazanium;2-hydroxy-2-oxoacetate
• 化学式: C₂O₄*2C₄H₁₂N
• 分子量: 236.312
• InChiKey: YDQRYONFUIGGGF-UHFFFAOYSA-N

计算性质

• 辛醇/水分配系数(LogP)：
  -0.23
• 重原子数：
  11
• 可旋转键数：
  3
• 环数：
  0.0
• sp3杂化的碳原子比例：
  0.67
• 拓扑面积：
  86.6
• 氢给体数：
  3
• 氢受体数：
  5

反应信息

• 作为反应物：
  描述：

  bis(diethylammonium) oxalate 、 碳酸二甲酯 在 1-ethyl-3-methylimidazolium bromide 作用下， 反应 8.0h， 以73.2%的产率得到Diethyl(dimethyl)azanium;oxalate
  参考文献：
  名称：

  咪唑基离子液体催化剂催化铵盐的烷基化

  摘要：

  在咪唑鎓离子液体催化剂上由铵盐和碳酸二烷基酯合成季铵盐。该反应产生了几乎化学计量的用于卤化物和硝酸盐的季铵盐。发现铵阳离子的烷基部分的供电子性，碳酸盐烷基的亲电子性质，铵盐的阴离子所对应的酸的酸度以及铵的空间位阻。盐和碳酸二烷基酯是影响季铵盐收率的关键因素。铵盐氮原子上的强供电子烷基，碳酸二烷基酯的亚甲基碳上的吸电子基团，

  DOI：

  10.1002/adsc.200600451

文献信息

• [EN] PROCESS FOR PREPARING TIOTROPIUM BROMIDE<br/>[FR] PROCÉDÉ POUR LA PRÉPARATION DE BROMURE DE TIOTROPIUM
  申请人：HOVIONE INT LTD

  公开号：WO2013117886A1

  公开（公告）日：2013-08-15

  The present invention relates to a novel process for the preparation of tiotropium bromide there is provided a process for preparing tiotropium bromide comprising (i) reacting scopine oxalate with diethylamine in an inert solvent to form scopine; (ii) reacting scopine and methyl di-(2-dithienyl)glycoIate (MDTG) in the presence of an inorganic base, and in an inert solvent to form N-demethyltiotropium; (iii) reacting N-demethyltiotropium with bromomethane in an inert solvent to form tiotropium bromide; (iv) crystallizing tiotropium bromide in a mixture of methanol and acetone, and optionally thereafter, (v) micronizing the tiotropium bromide so formed.

  本发明涉及一种用于制备噻托溴铵的新型工艺，提供了一种制备噻托溴铵的工艺，包括：(i) 在惰性溶剂中将斯可平草酸盐与二乙胺反应以形成斯可平；(ii) 在存在无机碱和惰性溶剂的条件下，将斯可平与二-(2-二硫代吡啶基)甘醇酸甲酯（MDTG）反应以形成N-去甲基噻托溴铵；(iii) 在惰性溶剂中将N-去甙基噻托溴铵与溴甲烷反应以形成噻托溴铵；(iv) 在甲醇和丙酮混合物中结晶化噻托溴铵，随后可选地，(v) 对所形成的噻托溴铵进行微粉化处理。
• Synthesis and structures of nickel(II) and copper(II) compounds of 5,5,7,13-tetramethyl-13-nitro-1,4,8,11-tetraazacyclotetradecane and the 13-ethyl-5,5,7-trimethyl-homologue
  作者：Neil F. Curtis、Kelly Flood、Ward T. Robinson、Joyce M. Waters

  DOI：10.1016/j.poly.2009.02.019

  日期：2009.7

  c-4-ene)-nickel(II) and -copper(II), and of their 13-ethyl-5,7,7-trimethyl-homologues, yield the nitro-substituted cyclic tetraamine cations (5,5,7,13-tetramethyl-13-nitro-1,4,8,11-tetraazacyclotetradecane)-nickel(II) and -copper(II), [M(neh)] 2+ , and (13-ethyl-5,5,7-trimethyl-homologues, [M(nph)] 2+ , respectively. The nickel(II) cations form square–planar, singlet ground, state salts with poorly

  用草酸盐形成链状聚合物链烯-反式-β-[Ni（neh）（μ-C2 O 4）] n·3 n（H 2 O）。形成折叠的大环化合物顺式-α-[Ni（neh）（C 5 H 7 O 2）] ClO 4和顺式-α-[Ni（neh）} 2（C 2 O 4）]（ClO 4）2螯合物为乙酰丙酮酸酯和草酸酯，构型为1 R，4 R，8 R，11R =α。它们与HClO 4反应，形成亚稳的α-[Ni（neh）]（ClO 4）2并保持构型。铜（II）阳离子与配位性差的阴离子形成深红色盐，以及与配位性阴离子形成深浅不一的蓝色的β-[Cu（neh）A] ClO 4型化合物。单峰基态方-平面镍（II）化合物的结构β-[Ni（neh）]（ClO 4）2·H 2 O，β-[Ni（neh）]（ClO 4）2，β-[Ni（ neh）] 2 [ZnCl 3（OH 2）] 2 [ZnCl 4]·H 2 O和α-[Ni（neh）]（ClO
• Composition for film formation, method of film formation, and silica-based film
  申请人：JSR CORPORATION

  公开号：US20030091838A1

  公开（公告）日：2003-05-15

  A composition for film formation which comprises: (A) a product of hydrolysis and condensation obtained by hydrolyzing and condensing at least one silane compound selected from the group consisting of compounds represented by the formula (1), compounds represented by the formula (2), and compounds represented by the formula (3) in the presence of water and an ammonium compound, and (B) an organic solvent.

  一种用于成膜的组合物，它包括 (A) 至少一种硅烷化合物的水解和缩合产物，该硅烷化合物选自由式（1）、式（2）和式（3）所代表的化合物组成的组，在水和铵化合物存在下水解和缩合得到，以及 (B) 有机溶剂。
• Compounds of nickel(II) with 5SR,7RS,12SR,14SR-5,12-dimethyl-7,14-diphenyl-1,4,8,11-tetraazacyclotetradecane, rmL2: The structures of [Ni(rmL2)](ClO4)2·0.5H2O and cis-[Ni(rmL2)(acac)]ClO4
  作者：Donald F. Cook、Neil F. Curtis、Clifton E.F. Rickard、Joyce M. Waters

  DOI：10.1016/j.poly.2005.06.022

  日期：2005.12

  The imine functions of [Ni(mL(1)])ClO4)(2) (mL(1) = meso-7RS,14SR-5,12-dimethyl-7,14-diphenyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene) are reduced by using NaBH4 in acetonitrile/methanol to form the meso-meso and rac-meso isomeric cyclic tetramine complex cations [Ni(mmL(2))](2+) and [Ni(mL(2))](2+) (mml(2) =5RS,7RS,12SR,14SR- and rmL(2) = 5SR,7RS, 12SR, 14SR-5,12-dimethyl-7,14-diphenyl-1,4,8,11-tetraazacyclotetradecane) in ca. 8:1 proportions. [Ni(rmL(2))](2+) is also prepared from rmL(2), formed in < 1% yield by the reduction of mL(1) by NaBH4 in ethanol. Square planar singlet ground state (S = 1) salts [Ni(rmL(2))](ClO4)(2) and [Ni(rmL(2))][ZnCl4] and triplet ground state (S=3) trans-di-ligand octahedral compounds trans-[Ni(rmL(2))X-2] (X- = Cl-,Br-,NCS- N-3(-) NO3-,NO2- and HCO3-), mu-Y-trans-[Ni(rmL(2))Y] (Y2- = C2O42- and [Ni(CN)(4)](2-)) and folded macrocycle compounds cis-[Ni(rmL)(acac)]ClO4 (acac(-) = pentane-2,4-dionato), cis-[Ni(rmL(2))}(2)(C2O4)](ClO4)(2), cis-[Ni(rmL(2))(H2O)(2)](ClO4)(2) and cis-[Ni(rmL(2))X-2], X- = Cl-, Br-, are described. The S=1 salt 1SR,4SR,5SR,7RS,8RS,11RS12SR,14SR-[Ni(rmL(2))]- (ClO4)(2) (.) 0.5H(2)O has a disordered structure with Ni(II) in square planar coordination by the nitrogen atoms of the macrocycle, in N-configuration III. with Ni-N-mean = 1.96(2) angstrom. The six-membered chelate rings both have chair conformations, with the phenyl substituents equatorially oriented and with the methyl substituents disordered over axial and equatorial orientations. The S = 3 compound cis-1SR,4SR,5SR,7RS,8SR,11SR,12SR,14SR-[Ni(rmL(2))(acac)]ClO4 has Ar-configuration V. The macrocycle is folded along N-1-Ni-N-8, adjacent to the phenyl substituents N1-Ni-N8 = 176.45(6) N4-Ni-N11 = 98.16(6)degrees}, with mean Ni-N = 2.09(2) angstrom and mean Ni-O = 2.121(5) angstrom. Both six-membered chelate rings have chair conformations with the methyl substituents equatorially oriented, while one has the phenyl substituent equatorially and the other has it axially oriented. The structures of the isomeric [M(rmL(2))(acac)ClO4, [M(rrL(2))(acac)]ClO4 and [M(mmL(2))(acac)]ClO4 compounds are compared. (c) 2005 Elsevier Ltd. All rights reserved.
• Nickel(II) compounds of a tri-amine mono-imine macrocycle: Preparations and structures of (5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradec-4-ene)nickel(II) compounds
  作者：Neil F. Curtis、Jan Wikaira

  DOI：10.1016/j.poly.2010.12.028

  日期：2011.3

  Reduction of one imine function of (5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradeca-4,11-diene)nickel(II) with 1 molar proportion of NaBH4 produces as the major product the tri-amine-monoimine macrocyclic cation (5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradec-4-ene)nickel(II), Ni(tm)](2+). Pairs of isomeric singlet ground state perchlorate and tetrachlorozincate salts of [Ni(tm)](2+) were prepared and the structures determined for the 1RS,8SR,11SR,12RS (labeled as beta) and 1RS,8RS,11RS,12SR (labeled as alpha) tetrachlorozincate salts. Triplet ground state trans-beta-[Ni(tm)(NCS)(2)] and catena-trans-beta-Ni(tm)-NC-Ni(CN)(2)-CN-}(n)center dot 2nH(2)O have the macrocycle in planar coordination and alpha-[Ni(tm)}(2)(C2O4)](ClO4)(2) has the macrocycle folded. With pentane-2,4-dione the compounds [beta-Ni(tm)]center dot[alpha-Ni(tm)(acac)](ClO4)(3) and [Ni(teta)]center dot[alpha-Ni(tm)(acac)](ClO4)(3) (teta = C-meso-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane) with both square-planar and octahedral Ni(II) cations were prepared and the latter was structurally characterized. Isomerisation in solution of metastable alpha-[Ni(tm)](2+) to stable beta-[Ni(tm)](2+) is extremely slow, even in base. (C) 2011 Elsevier Ltd. All rights reserved.