Showing papers in "Organic Process Research & Development in 2015"

TL;DR: In this paper, a multiauthor review article aims to bring readers up to date with some of the current trends in the field of process analytical technology (PAT) by summarizing each aspect of the subject (sensor development, PAT based process monitoring and control methods) and presenting applications both in industrial laboratories and in manufacture.

TL;DR: This review summarizes selected publications from Organic Process Research & Development using DoE to show how processes can be optimized efficiently and how DoE findings may be applied to scale-up.

TL;DR: Ruthenium(II) complexes have emerged as effective catalysts for C-H arylations of tetrazolyl-substituted arenes by chelation assistance.

TL;DR: Oscillatory flow reactors (OFRs) offer a suitable platform to deliver consistent operating conditions under plug-flow operation while maintaining a controlled steady state as discussed by the authors, which is an attractive approach for the delivery of consistent particles with specified critical quality attributes (CQAs).

TL;DR: Limiting oxygen concentration values, which define the minimum partial pressure of oxygen that supports a combustible mixture, have been measured for nine commonly used organic solvents at elevated temperatures and pressures to define safe operating conditions for the use of oxygen with organicsolvents.

TL;DR: In this paper, the authors investigated the scope and limitations of current methodology using standard laboratory techniques in an industrial context and identified several drawbacks with this approach, such as the high loading, poor turnover, and susceptibility to substrate inactivation of the catalysts.

TL;DR: A new paradigm for palladium-catalyzed, silicon-based cross-coupling reactions has been developed that employs a heretofore underutilized class of silicon reagents, the organosilanols, which represents an operationally simple and mild alternative to the fluoride-based activation method.

TL;DR: Asymmetric phase transfer catalysis has been recognized as an approach that is greener and more sustainable than synthetic alternatives and has evolved into one of the most practical methods in challenging enantioselective synthesis.

TL;DR: CSYNTH as discussed by the authors is a computer-aided synthesis design tool that predicts new ideas for route design to that of historical brainstorm results on a series of commercial pharmaceutical targets, as well as literature data.

TL;DR: The practical aspects of Cp*Rh(III)-catalyzed direct C-H amidation with 1,4,2-dioxazol-5-ones were investigated on the operational safety, use of green solvent, and scalability.

TL;DR: A survey of solvent usage for papers published in organic process research & development has been carried out for the years 1997-2012 as mentioned in this paper, where three solvent categories were studied: (i) solvents of concern, (ii) dipolar aprotic solvants, and (iii) neoteric solvent.

TL;DR: The IQ Consortium reports on the current state of process analytical technology (PAT) for active pharmaceutical ingredient (API) development in branded pharmaceutical companies as discussed by the authors, using an API process workflow (process steps from raw material identification through to finished API).

TL;DR: In this paper, a review highlights the recent achievements in replacing precious-metal-based catalysts with nonprecious-metal based catalysts in two important syntheses: hydroamination and C-N coupling reactions.

TL;DR: The addition of catalase, single-electron oxidants, and copper ions was investigated systematically in order to find the minimum concentrations required to obtain a fully active GOase.

TL;DR: A number of new, heterogeneously catalyzed processes to selectively oxidize alcohols into carbonyl or carboxyl compounds have been introduced in the past decade.

TL;DR: In this article, a spirocyclopropane-proline derivative at leaded bronze was scaled up in a divided batch-type electrolysis cell in good yield and excellent selectivity.

TL;DR: An improved Cu/nitroxyl catalyst system for aerobic alcohol oxidation has been developed for the oxidation of functionalized primary and secondary alcohols to aldehydes and ketones, suitable for implementation in batch and flow processes as mentioned in this paper.

TL;DR: The experimental application of an automated control strategy is presented for an end-to-end continuous pharmaceutical pilot plant and demonstrates that automated control can successfully keep critical material attributes close to the desired set points for a sustained period of operation.

TL;DR: In this paper, a continuously seeded l-glutamic acid cooling crystallization process, in a continuous oscillatory baffled crystallizer, was designed and operated to deliver control over polymorphic form.

TL;DR: In this paper, a large microflow electrolysis cell for laboratory synthesis on a multigram scale is described based on two circular electrodes with a diameter of 149 mm and a spiral electrolyte flow channel 2000 mm long, 5 mm wide, and 0.5 mm interelectrode gap.

TL;DR: In this paper, a systematic approach has been established to transfer an existing batch process enabling the implementation of a continuous process in an oscillatory baffled crystallizer (OBC) using ultrasound.

TL;DR: In this paper, the authors compare the effectiveness of Raman spectroscopy, particle vision and measurement (PVM), and infrared spectrograms to detect nucleation and polymorphic transformations during crystallization processes.

TL;DR: A scalable process to the insecticide Isoclast manufactured by Dow AgroSciences LLC is described, which involves the de novo construction of a fully elaborated pyridine sulfide using enamine-mediated cyclization followed by two efficient and inexpensive oxidations to introduce the sulfoximine.

TL;DR: In this article, a temperature-controlled aluminum plate microreactor was developed and tested in the exothermic synthesis of 3-piperidino propionic acid ethyl ester by Michael addition.

TL;DR: In this paper, the authors report the in-line formation and instantaneous consumption of Vilsmeier reagent utilizing both conventional batch and flow technologies and demonstrate the synthesis of Vildagliptin, thereby mitigating potential safety and hygiene hazards.

TL;DR: In this paper, the Ames data for 44 commercially available boronic acids and derivatives, including bis(pinacolato)diboron and bis-boronic acid, were provided.

TL;DR: In this article, the influence of crucial reaction parameters on Knoevenagel condensation in planetary ball mill was investigated and it was found that higher rotation frequency, lower dMB, milling beakers with larger diameter, and a ΦMB of ∼0.3 are advantageous for the reaction.

TL;DR: In this paper, a review aims to introduce the technique and highlight some examples where continuous preferential crystallization has been employed, emphasizing the advantages in process efficiency, including better process control and reproducibility with higher material throughput.

TL;DR: In this article, a tube-in-shell membrane flow reactor was developed for aerobic oxidation reactions that allowed continuous delivery of O2 to a liquid-phase reaction along the entire length of the flow path.

TL;DR: This account describes the laboratory's efforts in the development of a palladium-catalyzed asymmetric conjugate addition of arylboronic acids to cyclic conjugates acceptors and highlights the study of this transformation in the following areas: construction of all-carbon quaternary stereocenters, elucidation of the reaction mechanism, and so on.