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CAS No. : | 36822-11-4 | MDL No. : | MFCD00059166 |
Formula : | C10H8N2OS | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | XEKNACRTWJHOCE-UHFFFAOYSA-N |
M.W : | 204.25 | Pubchem ID : | 697057 |
Synonyms : |
6-Phenyl-2-thiouracil
|
Chemical Name : | 2-Mercapto-6-phenylpyrimidin-4-ol |
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280 | UN#: | N/A |
Hazard Statements: | H302-H312-H332 | Packing Group: | N/A |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrazine hydrate; for 4.0h;Reflux; | General procedure: A mixture of 6-(4-chlorophenyl)-3,4-dihydro-2-thiopyrimidin-4(3H)-one 8b (500mg, 2.1mmol) and hydrazine monohydrate (7.15mL, 7.36g, 0.15mol) was stirred at reflux for 4h. Afterwards, hydrazine was evaporated under reduced pressure. The residue was then triturated with water for 30min. The obtained precipitate was filtered off and subsequently washed with water to give a white powder used in the next step without further purification. 1H NMR (400MHz, DMSO-d6) delta ppm 6.11 (s, 1H, CH-pyrimidine ring), 7.49-7.51 (d, 2H, Ar), 7.98-8.01 (d, 2H, Ar), 8.57 (s, 1H, NH) |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
24% | With sodium ethanolate; In ethanol;Reflux; | To a solution of compound 12.1 (2 g, 10.41 mmol) in EtOH (15 mL) was added EtONa (7 mL, 18.7 mmol) and compound 1.2 (1.18 g, 15.61 mmol). Stirring was continued at reflux overnight. The solvent was removed under reduced pressure. The reaction was taken up with water, acidified to pH 3, extracted with EtOAc (3 x 20 mL) washed with brine and dried over Na2SO4.The crude was purified by flash chromatography, eluting with CH2C12/MeOH (2.5% for product) affording the title compound 12.2 (500 mg, 2.44 mmol) as white solid. Yield 24%. |
With sodium; In ethanol; for 12.0h;Reflux; | General procedure: Sodium metal (1.3g, 56.1mg-formula) was dissolved in 30mL of absolute ethanol, then thiourea (2.9g, 38.2mmol) and 4-bromobenzoylacetate (6.9g, 25.5mmol) were added in sequence to the clear solution. The mixture was heated at reflux for 12h. The resulting mixture was cooled at room temperature, the solvent was distilled in vacuo at 40-50C, and the residue was dissolved in a little amount of water to obtain a basic solution which was extracted with diethyl ether (2×50mL). The basic aqueous solution was acidified while cooling with ice bath to pH=2 to give a precipitate that was filtered and washed with water. The resulting compound was a white solid used in the next step without further purification. 1H NMR (400MHz, DMSO-d6) delta ppm 6.11 (s, 1H, CH-pyrimidine ring), 7.64-7.66 (d, 2H, Ar), 7.69-7.71 (d, 2H, Ar), 12.56 (s, 2H, NH). |
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