Prop-2-enyl 2,2-difluorobutanoate

• 分子结构分类: 有机化合物 - 脂质和类脂质分子 - 脂肪酰基
• 英文名称: Prop-2-enyl 2,2-difluorobutanoate
• 英文别名: prop-2-enyl 2,2-difluorobutanoate
• 化学式: C₇H₁₀F₂O₂
• 分子量: 164.15
• InChiKey: XPFPPGREUWHROR-UHFFFAOYSA-N

计算性质

• 辛醇/水分配系数(LogP)：
  2.3
• 重原子数：
  11
• 可旋转键数：
  5
• 环数：
  0.0
• sp3杂化的碳原子比例：
  0.57
• 拓扑面积：
  26.3
• 氢给体数：
  0
• 氢受体数：
  4

文献信息

• A PROCESS FOR THE PREPARATION OF ALKYL 3-DIFLUOROMETHYL-1-METHYL-1H-PYRAZOLE-4-CARBOXYLATE AND ITS ANALOGS
  申请人：KingChem LLC.

  公开号：US20150158808A1

  公开（公告）日：2015-06-11

  The disclosure provides a process for the preparation of alkyl 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylate and its analogs. The process includes a reaction workup method for Claisen condensation, wherein the enolate salt is acidified after removing remaining starting material and byproducts such as, ethanol and excessive ethyl acetate. The process also includes a method for completely drying alkyl difluoroacetoacetate and its analogs before use in the next step by reacting trialkyl orthoformate with the residual water. The process includes using Na 2 CO 3 and/or K 2 CO 3 to promote the ring-closure reaction to produce the alkyl 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylate. The process also includes effectively removing the regioisomer, alkyl 3-difluoromethyl-2-methyl-1H-pyrazole-4-carboxylate formed as a byproduct of the ring closure by a precipitation in a mixed solvent system and thereby eliminating the need for recrystallization of the final product.

  该披露提供了一种制备烷基3-二氟甲基-1-甲基-1H-吡唑-4-羧酸酯及其类似物的过程。该过程包括一种用于Claisen缩合的反应工作方法，其中在去除剩余的起始物质和副产物（如乙醇和过量的乙酸乙酯）后，使烯醇盐酸化。该过程还包括一种在下一步使用烷基二氟乙酰乙酸酯及其类似物之前完全干燥的方法，即通过将三烷基正甲酸酯与残留水反应。该过程包括使用Na2CO3和/或K2CO3促进环闭合反应，以产生烷基3-二氟甲基-1-甲基-1H-吡唑-4-羧酸酯。该过程还包括通过在混合溶剂体系中沉淀的方式有效去除环闭合的副产物烷基3-二氟甲基-2-甲基-1H-吡唑-4-羧酸酯，从而消除了对最终产品的再结晶的需要。
• [EN] PROCESS FOR PREPARING ALKYL 3-DIFLUOROMETHYL-1-METHYL-1H-PYRAZOLE-4-CARBOXYLATE AND ITS ANALOGS<br/>[FR] PROCÉDÉ DE PRÉPARATION DE 3-DIFLUOROMÉTHYL-1-MÉTHYL-1H-PYRAZOLE-4-CARBOXYLATE D'ALKYLE ET DE SES ANALOGUES
  申请人：KING CHEM LLC

  公开号：WO2015085464A1

  公开（公告）日：2015-06-18

  The disclosure provides a process for the preparation of alkyl 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylate and its analogs. The process includes a reaction workup method for Claisen condensation, wherein the enolate salt is acidified after removing remaining starting material and byproducts such as, ethanol and excessive ethyl acetate. The process also includes a method for completely drying alkyl difluoroacetoacetate and its analogs before use in the next step by reacting trialkyl orthoformate with the residual water. The process includes using Na2CO3 and /or K2CO3 to promote the ring-closure reaction to produce the alkyl 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylate. The process also includes effectively removing the regioisomer, alkyl 3-difluoromethyl-2-methyl-1H-pyrazole-4-caboxylate formed as a byproduct of the ring closure by a precipitation in a mixed solvent system and thereby eliminating the need for recrystallization of the final product.

  该披露提供了一种制备烷基3-二氟甲基-1-甲基-1H-吡唑-4-羧酸酯及其类似物的过程。该过程包括一种用于Claisen缩合的反应工作方法，其中在去除剩余的起始物质和副产物（如乙醇和过量的乙酸乙酯）后，使烯醇盐酸化。该过程还包括一种在下一步使用烷基二氟乙酮酸酯及其类似物之前完全干燥的方法，即通过将三烷基正甲酸酯与残留水反应。该过程包括使用Na2CO3和/或K2CO3促进环闭合反应，以产生烷基3-二氟甲基-1-甲基-1H-吡唑-4-羧酸酯。该过程还包括通过在混合溶剂系统中沉淀的方式有效地去除环闭合的副产物烷基3-二氟甲基-2-甲基-1H-吡唑-4-羧酸酯，从而消除了对最终产品的再结晶的需求。
• PREPARATION OF ALKYL 3-DIFLUOROMETHYL-1-METHYL-1H-PYRAZOLE-4-CARBOXYLIC ACID ESTER
  申请人：KingChem LLC

  公开号：US20140221669A1

  公开（公告）日：2014-08-07

  The present disclosure provides a novel and economically advantageous process for preparation of compounds of Formula I, such as alkyl 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid ester. The process includes acidification of the sodium enolate of alkyl difluoroacetoacetate by carbonic acid generated in situ by reacting carbon dioxide with water. The disclosure also includes promoting the ring closure reaction in which alkyl 2-alkomethylene-4,4-difluoro-3-oxobutyrate is reacted with methylhydrazine in two phase system with a weak base such as Na 2 CO 3 or K 2 CO 3 .

  本公开提供了一种新颖且经济优势的制备I型化合物的方法，例如烷基3-二氟甲基-1-甲基-1H-吡唑-4-羧酸酯。该方法包括通过在碳酸二气与水反应产生的碳酸酸化烷基二氟乙酰乙酸钠烯醇。本公开还包括促进环合反应，其中烷基2-烯丙基-4,4-二氟-3-酮丙酸酯与甲基肼在弱碱性的Na2CO3或K2CO3两相体系中反应。
• PROCESS FOR THE PREPARATION OF ALKYL 3-DIFLUOROMETHYL-1-METHYL-1H-PYRAZOLE-4-CARBOXYLATE AND ITS ANALOGS
  申请人：KingChem LLC.

  公开号：US20150353501A1

  公开（公告）日：2015-12-10

  The disclosure provides a process for the preparation of alkyl 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylate and its analogs. The process includes a reaction workup method for Claisen condensation, wherein the enolate salt is acidified after removing remaining starting material and byproducts such as, ethanol and excessive ethyl acetate. The process also includes a method for completely drying alkyl difluoroacetoacetate and its analogs before use in the next step by reacting trialkyl orthoformate with the residual water. The process includes using Na 2 CO 3 and/or K 2 CO 3 to promote the ring-closure reaction to produce the alkyl 3-di-fluoromethyl-1-methyl-1H-pyrazole-4- carboxylate. The process also includes effectively removing the regioisomer, alkyl 3-difluoro methyl-2-methyl-1H-pyrazole-4-carboxylate formed as a byproduct of the ring closure by a precipitation in a mixed solvent system and thereby eliminating the need for recrystallization of the final product.

  本公开提供一种制备烷基3-二氟甲基-1-甲基-1H-吡唑-4-羧酸酯及其类似物的方法。该方法包括一种Claisen缩合反应的反应工艺方法，其中在去除剩余的起始物和副产物（如乙醇和过量的乙酸乙酯）后酸化烯醇盐。该方法还包括一种在下一步使用烷基二氟乙酰乙酸酯及其类似物之前完全干燥的方法，即通过将三烷基正酯与残留水反应。该方法包括使用Na2CO3和/或K2CO3促进环合反应以产生烷基3-二氟甲基-1-甲基-1H-吡唑-4-羧酸酯。该方法还通过在混合溶剂体系中沉淀的方式有效地去除环合的副产物烷基3-二氟甲基-2-甲基-1H-吡唑-4-羧酸酯的异构体，从而消除了对最终产品的再结晶的需要。
• US8871947B2
  申请人：——

  公开号：US8871947B2

  公开（公告）日：2014-10-28