ChemicalBook CAS DataBase List 5-NITROTHIOPHENE-2-CARBOXALDEHYDE

5-NITROTHIOPHENE-2-CARBOXALDEHYDE synthesis

13synthesis methods

Product Name:5-NITROTHIOPHENE-2-CARBOXALDEHYDE
CAS Number:4521-33-9
Molecular formula:C5H3NO3S
Molecular Weight:157.15

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Yield:4521-33-9 80%

Reaction Conditions:

with hydrogenchloride in methanol;water at 65; for 8 h;

Steps:

1.2; 1.3; 2.2; 2.3; 3.2; 3.3

(2) In a 250 mL four-neck flask, add 16 g of water and 71 g of methanol. Under stirring, add 7.5 g of the wet 5-nitrothiophen-2-ylmethylene diacetate obtained in step (1), and keep Under stirring conditions, 7.2g hydrochloric acid was added dropwise; refluxed at 65°C for 8 hours to prepare a reaction solution; the resulting reaction solution was naturally cooled to 30°C, 40 mL of water was added, stirred, and cooling continued to precipitate solids and filtered to obtain 5-nitrothiophene-2-carbaldehyde 6g;(3) In a 250mL four-necked flask, add the result of step (2) 6g of 5-nitrothiophene-2-carboxaldehyde, 15.8g of methanol, heated to 65°C, refluxed for 1h to prepare a reaction liquid; under stirring conditions, add 6.6g of n-hexane to the obtained reaction liquid, and cool to -5°C The solids are separated out, filtered and dried to obtain 5-nitro-2-thiophenecarboxaldehyde 4g, purity 99.3%, yield 80%.

References:

CN112939929,2021,A Location in patent:Paragraph 0035; 0037-0039; 0041-0043; 0045-0046

98-03-3 Synthesis