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68925-98-4

3-Nitrodibenzothiophene-5-oxide synthesis

3synthesis methods
-

Yield:68925-98-4 87%

Reaction Conditions:

with sulfuric acid;nitric acid;acetic acid in water at 0 - 5; for 1 h;Inert atmosphere;

Steps:

13 [237] Preparation Example 13. Synthesis of Intermediate 13 (3- nitrobenzothiophene5-oxide)

[239] In a 500 ml round-bottom three-neck flask under a nitrogen atmosphere, 16.8 g of Intermediate 11, 58.8 g of acetic acid and 199 g of sulfuric acid were placed, and maintained at 0°C. 18 g of 70% nitric acid solution was slowly added dropwise and stirred below 5°C for 1 hr. After completion of the reaction, water was added, crystal was formed, filtered, thus obtaining 18.0 g of Intermediate 13 (yield 87%).[240] MS (ESI): [M+H]+ 246

References:

WO2017/196081,2017,A1 Location in patent:Paragraph 237; 238; 239; 240