1,2-Dibenzoylthiosemicarbazide
Round 1
Reviewer 1 Report
Comments and Suggestions for AuthorsThis paper primarily describes the benzoylation reaction starting from thiosemicarbazide (1) to afford the title compound, 1,2-dibenzoylthiosemicarbazide (3). The authors demonstrated the benzoylation of thiosemicarbazide (1) and 1-benzoylthiosemicarbazide (2) under two different base conditions, which were summarized in Tables 1 and 2. These results illustrated the benzoylation of thiosemicarbazide (1) through 1-benzoylthiosemicarbazide (2). The reviewer feels that the results are worthy of publication in this Journal. However, the reviewer will recommend some revisions of the manuscript before the publication.
Table 2 should be benzoylation of 1-benzoylthiosemicarbazide (1).
Column 1 in Table 2 has also been revised from (1) to (2).
Line 71. Monobenzoylation of 1 is not an unexpected result.
Line 75. Exclusive formation does not seem to be a unique phenomenon for this reaction.
I think accurate notation is necessary.
4. Experimental. Tables 1 and 2 seem to be the results of HPLC, but they do not seem to be consistent with the practical synthesis.
1-Benzoylthiosemicarbazide (2) was obtained almost quantitatively, but the yield was 32%.
1,2-Dibenzoylthiosemicarbazide (3) was obtained in 62% yield from 1, but the Table 1 shows much lower yield.
Author Response
Table 2 should be benzoylation of 1-benzoylthiosemicarbazide (1). v
Column 1 in Table 2 has also been revised from (1) to (2). V
“We replaced in Table 2 thiosemicarbazide with 1-benzoylthiosemicarbazide (2) and also inside the table (1) with (2).”
Line 71. Monobenzoylation of 1 is not an unexpected result.
We replaced with “and also the formation of monobenzoylation product when starting from thiosemicarbazide (1)”
Line 75. Exclusive formation does not seem to be a unique phenomenon for this reaction.
“Exclusive was replaced with majoriy.”
I think accurate notation is necessary.
- Experimental. Tables 1 and 2 seem to be the results of HPLC, but they do not seem to be consistent with the practical synthesis.
1-Benzoylthiosemicarbazide (2) was obtained almost quantitatively, but the yield was 32%.
“It was a typo, thank you. The yield after recrystallization from methanol of 1-Benzoylthiosemicarbazide (2) was actually 62%. According to the HPLC analysis, the conversion is over 99%, but after isolation and purification by recrystallization, the yield is much lower. We replaced the correct value in the manuscript.”
1,2-Dibenzoylthiosemicarbazide (3) was obtained in 62% yield from 1, but the Table 1 shows much lower yield.
“It was a typo, thank you. The yield of 1,2-Dibenzoylthiosemicarbazide (3) from thiosemicarbazide (1) with 2 equivalents of benzoyl chloride in DMF, after recrystallization from acetonitrile, was actually 42%. We replaced the correct value in the manuscript.”