Benzoic acid, 3-mercapto-2-methyl- synthesis
- Product Name:Benzoic acid, 3-mercapto-2-methyl-
- CAS Number:188700-62-1
- Molecular formula:C8H8O2S
- Molecular Weight:168.21
![Benzoic acid, 3-[(ethoxythioxomethyl)thio]-2-methyl-](/CAS/20210305/GIF/1149388-17-9.gif)
1149388-17-9
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188700-62-1
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Yield:188700-62-1 99%
Reaction Conditions:
Stage #1: 3-{[(ethyloxy)carbonothioyl]thio}-2-methylbenzoic acidwith sodium hydroxide;water for 15 h;Heating / reflux;
Stage #2: with hydrogenchloride in water; pH=2;
Steps:
33.2
STEP 2: 3-{[(ethyloxy)carbonothioyl]thio}-2-methylbenzoic acid (270 mg, 1.05 mmol) in a IN aqueous sodium hydroxide solution (3 mL) was stirred at reflux for 15 hours. The mixture was cooled to room temperature and the pH was adjusted to 2 using concentrated aqueous hydrochloric acid. The aqueous mixture was extracted twice using dichloromethane and the combined organic solutions were washed with brine, then dried over anhydrous sodium sulfate. Filtration and concentration afforded 180 mg, 1.05 mmol (99%) of 3-mercapto-2-methylbenzoic acid. 1H NMR (400 MHz, CDCl3): 7.87 (d, IH), 7.47 (d, IH), 7.16-7.1 1 (m, IH), 3.43 (s, IH), 2.62 (s, 3H).
References:
WO2009/55077,2009,A1 Location in patent:Page/Page column 400
631416-27-8
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