5-ACETYLTHIOPHENE-2-CARBOXAMIDE synthesis
- Product Name:5-ACETYLTHIOPHENE-2-CARBOXAMIDE
- CAS Number:68257-89-6
- Molecular formula:C7H7NO2S
- Molecular Weight:169.2
4066-41-5
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Yield:68257-89-6 95.15%
Reaction Conditions:
Stage #1: 5-acetylthiophene-2-carboxylic acidwith oxalyl dichloride in N,N-dimethyl-formamide at 0 - 40;Inert atmosphere;Large scale;
Stage #2: with ammonia in acetonitrile;Large scale;Temperature;Solvent;
Steps:
1.a-3.a (a) Preparation of Intermediate I:
115g of 5-acetyl-thiophene-2-carboxylic acid was suspended in 1524g of acetonitrile, 2.3g of N,N-dimethylformamide was added, and after nitrogen replacement, the temperature was lowered to 0°C with stirring, and 128.9g of oxalyl chloride was slowly added. After the addition was completed, the temperature was slowly raised to 30-40°C and stirred. After the reaction was completed, the reaction solution was concentrated to dryness under reduced pressure. 1524 g of acetonitrile was added to the residue, and after stirring to dissolve completely, it was used for later use. 1.15L of concentrated ammonia water was added to the reaction kettle, the temperature was lowered to 15-25°C, and the acetonitrile solution of the above-mentioned intermediate state-acyl chloride was slowly added. After adding, filter and rinse the filter cake with water. After drying under reduced pressure, 108.8 kg of Intermediate I was obtained, the yield was 95.15%, and the HPLC purity was 98.78%.
References:
CN114773312,2022,A Location in patent:Paragraph 0042-0045; 0049-0051; 0054-0056
4101-81-9
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88-15-3
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114773-97-6
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