4-Fluoro-2-mercaptobenzoic acid synthesis
- Product Name:4-Fluoro-2-mercaptobenzoic acid
- CAS Number:81223-43-0
- Molecular formula:C7H5FO2S
- Molecular Weight:172.18
![Ethanamine, N-[(3,5-dichlorophenyl)methylene]-2,2-diethoxy-](/CAS/20210305/GIF/1000210-73-0.gif)
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Yield: 87%
Reaction Conditions:
Stage #1:methyl 2-((dimethylcarbamoyl)thio)-4-fluorobenzoate with sodium hydroxide at 100; for 14 h;
Stage #2: with hydrogenchloride; pH=3
Steps:
50 Reference Example 50
Reference Example 50 4-Fluorothisalicylic acid A mixture of methyl 2- [[(dimethylamino)carbonyl]thio]-4-fluorobenzoate (4.7 g, 18 mmol) and 10 % aqueous sodium hydroxide solution (36 g, 90 mmol) was stirred at 100 °C for 14 hrs.. The reaction mixture was acidified (PH 3) by the addition of 6 N hydrochloric acid, and the precipitates were collected.. The precipitates were dissolved in ethyl acetate, dried over anhydrous magnesium sulfate.. The solvent was evaporated to give the titled compound (2.7 g, 87 %) as pale yellow crystals.1H-NMR (CDCl3+DMSO-d6) δ: 5.50 (1H, br s), 6.83 (1H, m), 7.02 (1H, dd, J = 2.5, 9.3 Hz), 8.10 (1H, m).
References:
Takeda Chemical Industries, Ltd. EP1424336, 2004, A1 Location in patent:Page 133
937245-29-9
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