1,2-Dibenzoylthiosemicarbazide

Round 1

Reviewer 1 Report

 This 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.

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%.

“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.”