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CAS No. : | 15568-85-1 | MDL No. : | MFCD00599240 |
Formula : | C8H10O5 | Boiling Point : | - |
Linear Structure Formula : | CH3OCHCCOCOO2C(CH3)2 | InChI Key : | DVLSQHLXPRYYRC-UHFFFAOYSA-N |
M.W : | 186.16 | Pubchem ID : | 152111 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P264-P270-P301+P312-P330 | UN#: | N/A |
Hazard Statements: | H302 | 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 |
---|---|---|
In tetrahydrofuran; | Example N. 6 Preparation of 5- [1-(6-fluoro-2-methyl-1,2,3,4-tetrahydroquinolyl) ] -methylene-2,2-dimethyl 1,3-dioxan-4,6-dione 1.65 g (10 mmole) of 6-fluoro-2-methyl-1,2-3,4-tetrahydroquinoline and 2,05 g (11 mmole) of 2,2-dimethyl-5-methoxymethylene-1,3-dioxan-4,6-dione [prepared according to Monatshafte fuer Chemie, 98 , 565 (1967)] are reached under stirring and heating at 100-110C for 1 hour. The cooled reaction mass is taken up in tetrahydrofurane and the solids are filtered and dried. Yield: 2.5 g m.p.: 163-5C Flumequine is prepared from the resulting product according to the procedure of Example 1b. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
In isopropyl alcohol; at 80℃; for 0.166667h; | The 4-chloro-7-(N-methylcarbamoyl)quinoline used as starting material was prepared as <n="177"/>follows :-5-Methoxymethylene-2,2-dimethyl-l,3-dioxane-4,6-dione (3.24 g) was added to a stirred mixture of <strong>[120100-15-4]methyl 3-amino-2-chlorobenzoate</strong> (US Patent No. 6,177,440, columns 227 and 228 thereof; 3.1 g) and isopropanol (75 ml) and the resultant mixture was heated to 80C for 10 minutes. The reaction mixture was cooled to ambient temperature and the precipitate was recovered, washed with diethyl ether and dried under vacuum. There was thus obtained 5-(2-chloro-3-methoxycarbonylanilinomethylene)-2,2-dimethyl- 1 ,3-dioxane-4,6-dione (5 g); 1H NMR: (DMSOd6); 1.7 (s, 6H), 3.89 (s, 3H), 7.56 (m, IH), 7.67 (d, IH), 8.11 (br m, IH), 8.79 (br m, IH); Mass Spectrum: M+H+ 340. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
23% | 2-Bromomethyl-1-methoxy-4-nitrobenzene (2.03 g) was dissolved in N,N-dimethylformamide (30 ml). Triethylamine (5 ml) and 20% palladium hydroxide (1.08 g) were added to the solution, and the mixture was stirred under a hydrogen gas atmosphere at room temperature overnight. The reaction mixture was filtered and was then washed with chloroform. The solvent was removed by distillation under the reduced pressure, water was added to the residue, and the organic layer was extracted with ethyl acetate. The ethyl acetate layer was then washed with water and saturated brine and was dried over anhydrous sodium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue as such was used in the next reaction without purification. The residue and 5-methoxymethylene-2,2-dimethyl-[1,3]dioxan-4,6-dione (2.00 g) were suspended in 2-propanol (40 ml), and the suspension was stirred at 70C for 30 min. The reaction mixture was cooled to room temperature, and the precipitated crystal was then collected by filtration and was washed with methanol and then with ether. The crystal thus obtained as such was used in the next reaction without further purification. The crystal prepared above and biphenyl (5.9 g) were suspended in diphenyl ether (15 ml), and the suspension was stirred at 220C for 3 hr. The reaction mixture was cooled to room temperature, and the cooled reaction mixture as such was purified by column chromatography with an ethyl acetate-hexane system to give 6-methoxy-7-methyl-1H-quinolin-4-one (352 mg, yield 23%) (3 steps). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
99% | In isopropyl alcohol; at 25℃; for 2h; | To a suspension of 5-methoxymethylene-2,2-dimethyl-[1 ,3]dioxane-4,6-dione (31.1 g; 166.8 mmol) in isopropanol (800 mL) is added <strong>[2247-88-3]3-fluoro-pyridin-4-ylamine</strong> F-5b (17.0 g; 151 .6 mmol) portion wise and stirred at 25 °C for 2 h. The precipitated solid is filtered off and washed with isopropanol and diethyl ether. Afterwards 5-[(3-fluoro-pyridin-4-ylamino)- methylene]-2,2-dimethyl-[1 ,3]dioxane-4,6-dione F-6b is dried under reduced pressure. Yield: 99 percent (40.0 g; 150.3 mmol) To a suspension of 5-methoxymethylene-2,2-dimethyl-[1 ,3]dioxane-4,6-dione (31.1 g; 166.8 mmol) in isopropanol (800 mL) is added <strong>[2247-88-3]3-fluoro-pyridin-4-ylamine</strong> F-5b (17.0 g; 151 .6 mmol) portion wise and stirred at 25 °C for 2 h. The precipitated solid is filtered off and washed with isopropanol and diethyl ether. Afterwards 5-[(3-fluoro-pyridin-4-ylamino)- methylene]-2,2-dimethyl-[1 ,3]dioxane-4,6-dione F-6b is dried under reduced pressure. (0642) Yield: 99 percent (40.0 g; 150.3 mmol)To a suspension of 5-methoxymethylene-2,2-dimethyl-[1 ,3]dioxane-4,6-dione (31.1 g; 166.8 mmol) in isopropanol (800 mL) is added <strong>[2247-88-3]3-fluoro-pyridin-4-ylamine</strong> F-5b (17.0 g; 151 .6 mmol) portion wise and stirred at 25 °C for 2 h. The precipitated solid is filtered off and washed with isopropanol and diethyl ether. Afterwards 5-[(3-fluoro-pyridin-4-ylamino)- methylene]-2,2-dimethyl-[1 ,3]dioxane-4,6-dione F-6b is dried under reduced pressure. |
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