3-[(THIEN-2-YLCARBONYL)AMINO]BENZOIC ACID synthesis
- Product Name:3-[(THIEN-2-YLCARBONYL)AMINO]BENZOIC ACID
- CAS Number:24341-72-8
- Molecular formula:C12H9NO3S
- Molecular Weight:247.27
Yield:24341-72-8 95%
Reaction Conditions:
Stage #1: 2-thiophenylcarboxylic acidwith thionyl chloride for 1 h;Reflux;
Stage #2: meta-aminobenzoic acidwith triethylamine at 20; for 2 h;
Steps:
1.A
Step A: thiophene-2-carboxylic acid (1.024 g, 8 mmol) added 25 ml single-port in the bottle, by adding thionylchloride (5 ml), heated to reflux reaction for 1 hour. After the reaction pressure to remove thionyl chloride, oil pump and a ground line, adding anhydrous tetrahydrofuran is dissolved, slowly dissolved into the anhydrous tetrahydrofuran for 3 - aminobenzoic acid (1 a) (1.097 g, 8 mmol) and triethylamine (0.808 g, 8 mmol), the reaction at room temperature for 2 hours. After the reaction under reduced pressure to remove tetrahydrofuran, after the residue water 10 ml ethyl acetate 3 times, the organic phase for 10 ml saturated salt water washing 3 times, the organic phase under reduced pressure after the removal of the ethyl acetate, oil pump and a ground line to obtain white solid 3-(thiophene-2-amido)benzoic acid (2 a), yield 95%.
References:
CN108864038,2018,A Location in patent:Paragraph 0030