It is a deuterated compound and a member of chloromethanes. The deuterium signal is used for locking the spectrometer. because we typically want to observe protons, we use a solvent such as d-"chloroform" or d_6-"benzene", i.e. Concerning the proposed mechanism, are there any experimental evidences for this mechanism? 4. Water contamination can be a problem for deuterated NMR solvents. Magnetic Resonance in Chemistry In the introduction (page 2, lines 4 and 5) the authors justify the interest of deuterated solvents and CDCl3 in particular, due to their use as a solvents for NMR, but they present as references two papers concerning the deuteration of organic molecules (ref 2 and 3). The manuscript was thoroughly revised and all the concerns raised have been answered, either through the addition of new references and/or clarification of the text/discussion or by the addition of new experimental results as suggested by the reviewers. The authors would like to apologize about them. CDCl3 is an important chemical for various applications beside its use as NMR solvent. Another aspect of the introduction that needs to be reinforced is concerning the methodologies to prepare deuterated solvents (page 2 lines 8-12). It has a role as a non-polar solvent. Yours sincerely Dr. Teodor Parella Editor, Magnetic Resonance in Chemistry teodor.parella@uab.cat Referees' Comments: Reviewer: 1 Comments to the Author In the revised version of the paper by Higuera-Padilla et al concerning the NMR study of the catalytic activity for two ruthenium complexes for the production of deuterated chloroform using chloroform and deuterated water in KOH, the authors have addressed all the reviewers comments. We agreed with the reviewer and we added new information about CDCl3 production methods and respective references.P age 2, lines 14-22.3. Please do not submit the revised manuscript as a new manuscript. The reports of the referees are included at the foot of this EMAIL or as an attachment. [citation needed]. Higuera-Padilla, Angel Ruben; Besides, the experimental section was revised, leaving clear the procedures used for reaching the results showed on the figure 2, in consonance to written in the page 7, lines 8-20. Deuterated chloroform, 3 is most commonly used because of its low price. I would expect at least reference to the main methodology currently being used to prepare CDCl3 by commercial companies. Also please don't use this sub to cheat on your exams!! Can compound B be independently prepared to see if it is an intermediary of the deuteration of chloform?Other comments:Revision concerning English spelling and some typos:Page 1, line 19 – “demonstrated to be less efficient than compound A, which has”Line 25 – deuterated labelled Page 2, line 4 – “such as chloroform (CDCl3, 99,8%), despite having” “ are widely used as solvents in NMR”Line 10 – “friendly catalytic approach monitored in situ by NMR spectroscopy”Line 20 – “ was monitored in situ by 13C NMR…”, The communication by Higuera-Padilla et al describes the NMR study of the catalytic activity for two ruthenium complexes for the production of deuterated chloroform using chloroform and deuterated water in KOH.While I found that the findings reported in the communication are interesting and supported by the experimental data presented I missed a more exhaustive literature support that could justify the relevance of the work and some more discussion concerning the proposed mechanism (see bellow, detailed comments). In addition, the initial CHCl3:D2O was left clear, on this revised version in the page 3, lines 16-18. Deuterated chloroform (CDCl 3), also known as chloroform-d, is an isotopologue of chloroform (CHCl 3) in which the hydrogen atom ("H") is replaced with a deuterium (heavy hydrogen) isotope ("D"). Please note that in your revision of the manuscript, it is imperative to get everything correct. Your revised manuscript is due on: 24-Jun-2020 If you would like help with English language editing, or other article preparation support, Wiley Editing Services offers expert help with English Language Editing, as well as translation, manuscript formatting, and figure formatting at www.wileyauthors.com/eeo/preparation. The reaction using 0.01 mmol of compound A reached approximately 55% of H/D conversion in 1 h. In the same time, the reactions with 0.002 mmol of compound A and without catalyst show approximately 28% and 3% H/D exchange, respectively. They resonate at different frequencies that the probe isn’t currently “listening for” hence they don’t interfere unless they actually couple to your nuclei of interest and have sufficiently abundant spin-active nuclei for example if you made 13CHCl3 your proton spectrum would be a doublet due to the 13C coupling. It is not clear from the experimental section how the experiments in figure 2 were executed.We agreed with the reviewer and improved the discussions as shown in page 4, lines 21-25 and page 5, lines 1-3. The exchange between D and H was monitored by in situ NMR spectroscopy. Please do not submit the revised manuscript as a new manuscript. Batista, Alzir Azevedo; In proton NMR spectroscopy, deuterated solvent (enriched to >99% deuterium) must be used to avoid recording a large interfering signal or signals from the proton(s) (i.e., hydrogen-1) present in the solvent itself. Deuterated chloroform (CDCl 3), also known as chloroform-d, is an isotopologue of chloroform (CHCl 3) in which the hydrogen atom ("H") is replaced with a deuterium (heavy hydrogen) isotope ("D"). The exchange between D and H was monitored by in situ NMR spectroscopy. 2.1. Commercial chloroform-d does, however, still contains a small amount (0.2% or less) of non-deuterated chloroform; this results in a small singlet at 7.26 ppm, known as the residual solvent peak, which is frequently used as an internal chemical shift reference. CDCl3 is an important chemical for various applicatiooons beside its use as NMR solvent. Kock, Flavio Vinicius Crizostomo; Line 10 – “friendly catalytic approach monitored in situ by NMR spectroscopy”. New comments cannot be posted and votes cannot be cast. It is used because most compounds will dissolve in it, it is volatile and therefore easy to get rid of, and it is non-reactive and will not exchange its deuterium with protons in the molecule being studied. NMR SOLVENTS Deuterated Solvents for NMR • NMR Solvents • NMR Reference Standards • NMR Tubes. What was the actual CHCl3:D2O ratio?Concerning the proposed mechanism, are there any experimental evidences for this mechanism? The authors would like so much by your considerations about our researcher, them were totally pertinent.5. In addition, modern instruments usually require the presence of deuterated solvent, as the field frequency is locked using the deuterium signal of the solvent to prevent frequency drift. Carbon (or chlorine, phosphorus, etc) in the same magnet will resonate at 75 MHz (etc etc), in other words extremely far away from hydrogen, so you don't detect them all at the same time. 4. I would expect at least reference to the main methodology currently being used to prepare CDCl3 by commercial companies. It is the responsibility of the authors to supply any necessary permissions to the editorial office. I believe that the use of deuterated solvents and CDCl3 as an NMR solvent for routine analysis must be better justified and with more appropriate references.We agreed with the reviewer add more information about the relevance of the use of deuterated solvents, specially the CDCl3 on NMR analysis. Can compound B be independently prepared to see if it is an intermediary of the deuteration of chloform?Other comments:Revision concerning English spelling and some typos:Page 1, line 19 – “demonstrated to be less efficient than compound A, which has”Line 25 – deuterated labelled Page 2, line 4 – “such as chloroform (CDCl3, 99,8%), despite having” “ are widely used as solvents in NMR”Line 10 – “friendly catalytic approach monitored in situ by NMR spectroscopy”Line 20 – “ was monitored in situ by 13C NMR…”. You can also view these reports via your Author Center in ScholarOne Manuscripts. You can use this direct link: PLEASE NOTE: This is a two-step process. Journal: Materials Article Title: Analysis of Polycyclic Aromatic Hydrocarbon (PAH) Mixtures Using Diffusion-Ordered NMR Spectroscopy and Adsorption by Powdered Activated Carbon and Biochar doi: 10.3390/ma11040460 Figure Lengend Snippet: 1 H nuclear magnetic resonance (NMR) spectra and peak assignments in Deuterated chloroform (CDCl 3 ) of benzene, fluoranthene, 1,2-benzanthracene, … All the references should be in the proper format. You can upload your revised manuscript and submit it through your Author Center on MRC-ScholarOne Manuscripts. The title of the manuscript needs to be revised.2. Published in Therefore, more expensive alternatives like dichloromethane-d2 or benzene-d6 must be used if the analyte is expected to be highly acid-sensitive. As the reported H/D exchange protocol is limited to CHCl3 only and the use of RCH3 shows that this reaction is applicable for the deuteration of benzylic protons.3. The referees have recommended publication, but also suggest some minor revisions to your manuscript. NMR chemical shifts are a small correction on the basic frequency of hydrogen in a magnet, that's why they're quoted in ppm. Therefore, compound A is an efficient catalyst for a rapid and straightforward synthesis of CDCl(3)from CHCl(3)at room temperature and using D2O as deuterium source. This needs to be clarified in the figure and in the experimental section. However there is no attempt to explain why or to rationalize how the structural modification of the catalyst is influencing the activity. [citation needed], The properties of CDCl3 are virtually identical to those of regular chloroform, although biologically, it is slightly less toxic to the liver than CHCl3, due to its C–D bond, which is stronger than a C–H bond, making it somewhat less prone to form the destructive trichloromethyl radical (•CCl3).[5]. After the isolation of the chloroform fraction and two more addition of D2O, it was possible to obtain 95.0% H/D exchange in approximately 3 h, using 0.01 mmol of the compound A. substituted by deuteriums; these “deuterated” solvents have no interfering NMR absorptions. CDCl3 is a common solvent used for NMR analysis. Cambridge Isotope Laboratories, Inc. www.isotope.com s ... Chloroform-d (D,99.8%) DLM-7 [865-49-6] UN# 1888 No stabilizers are used in this product. For the compound B, 55% of H/D exchange conversion was achieved only in 1 hour, only when 0.05 mmol was used, that is a much higher catalyst concentration" change the position of "only"Line 23 – add has “complex A (cis-[RuCl2(dppb)(bipy)]) has”Line 25 – delete “the” and add “has” “the other hand, the complex B ([6-(p-cymene)Ru(dppb)Cl]PF6) has a tetrahedral geometry,”Page 5Line 2 - replace “cloudy” by “bulky”Page 6Line 4 – add “into” “A, as catalyst.
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