6,6′-Di-(2″-thiophenol)-2,2′-bipyridine
Round 1
Reviewer 1 Report
Comments to manuscript id: molbank-1644935
The short note submitted by Yan Huang and Lianpeng Tong is recommended for publication in Molbank. Before acceptance, I recommend the following major and minor edits:
- Authors should mention that a patent reports the platinum(II) complex of the ligand described herein: JP2010135689 A 2010-06-17
- Authors may point out that the respective 1,10-phenanthroline analogue is literature known: Lett. 2016, 18, 7, 1562–1565
- Please note that providing high resolution MS data does not prove sample purity. So please include elemental analysis for compounds 1 and 2.
Line 31: catalyzes electrochemical
Line 39: please specify “great” in “has great potential”
Line 91: atmospheric pressure
Line 118: please revise “…was stirred under Ar atmosphere until no gas bubble evolution.”
Line 130: Please revise as this statement is not covered by any evidence given in the manuscript: “It can be used as a novel tetradentate ligand to construct Ni complexes that mimic the active site of [NiFe]-hydrogenases.”
Line 131: Afore comment also applies to statement “We are currently preparing derivatives of 2 with various substituents via the synthetic route described herein” that lacks relevant information to readers.
Figures S2 and S4: It should read “13C{1H} NMR spectrum”
Author Response
"Please see the attachment.
Author Response File: 
Author Response.pdf
Reviewer 2 Report
This manuscript by Huang and Tong is dealing with the synthesis of dithiol-substituted bipyridyl. The original idea, synthesis, and characterizations were described in the manuscript with concise fashion. However, at the same time, I can see some insufficient data for structural confirmation of the final compound 2. Therefore, I suggest the major revision process before making final decision.
1) HR-MS or EA for compound 2 MUST BE PRESENTED. Since both compounds 1 and 2 are newly obtained and reported by this study. The final characterization of organic compound is the author’s duty. I cannot accept the new structure of organic molecule without HR-MS or elemental analysis (EA).
2) Direct evidence or proper references are significantly required for Ni-metalation under UV-Vis study. I cannot 100% guarantee for UV-Vis change in Figure 1(b) (from red to blue), without control experiments and related references.
3) FT-IR data for both compounds 1 and 2 are required to check newly introduced S-H bonds in compound 2.
4) Huge H2O peaks in 1H NMR of compound 1 and DCM in 1H NMR of compound 2 is not in acceptable size. Both NMRs should be remeasured and updated after purification.
5) Typo: Caption for Scheme 1, last period is not necessary.
6) There is no section 4; 2. Results and Discussion -> 4. Materials and Methods
7) Page 3, 170oC -> 170 oC
8) Page 4, 200oC -> 200 oC
Author Response
Please see the attachment.
Author Response File: Author Response.pdf
Round 2
Reviewer 2 Report
Additional Suggestions
1) for NMR, the description for difficulties on sampling of 1 and 2 (residual solvent and volatile properties) should be displayed in the supporting information (ideally in the caption for Figures S3 and S4)
2) For elemental analysis, 2-0.6H2O looks weird. The calculated portion of pure molecule 2 should be suggested, and the rationalization for 0.6 equivalent H2O should be confirmed by integral information from 1H NMR (Figure S4).
3) For FT-IR, the author should leave S-H sign at the peak near 2500 cm-1. It should be better for general audience of Mol. Bank.
Author Response
Please see the attachment.
Author Response File: Author Response.pdf
