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CAS No. : | 146137-78-2 | MDL No. : | MFCD00061311 |
Formula : | C8H4F4O | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 192.11 | Pubchem ID : | - |
Synonyms : |
|
Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-H335 | Packing Group: | |
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 potassium carbonate; In N,N-dimethyl-formamide; at 60℃; for 2h; | Production Example 1; A mixture of 5.0 g of 2-fluoro-5- ( trifluoromethyl ) benzaldehyde, 3.3 g of methyl thioglycolate , 4.0 g of potassium carbonate and 50 ml of DMF was stirred at 60C for 2 hours, and then the reaction mixture was cooled . to room temperature. To the reaction mixture was added water, and extracted with tert-butyl methyl ether 3 times. The combined organic layer was washed with water, followed by saturated aqueous sodium chloride solution. The mixture was dried over magnesium sulfate, and then concentrated under reduced pressure. The residue was recrystallized from methanol to obtain 6.3 g of methyl 5- ( trifluoromethyl ) benzo[ b] thiophene-2- carboxylate (the present compound 1) .[ The present compound 1]1 H-N R ( CDCI3 ) δ: 8.16(s, ' 1H) , 8.13(s, 1H) , 7.99(d, J=8.7Hz, 1H) , 7.67(d, J=8.7Hz, 1H) , 3.98(s, 3H) | |
With potassium carbonate; In N,N-dimethyl-formamide; at 60℃; for 2h; | Production Example 1; A mixture of 5.0 g of 2-fluoro-5- ( trifluoromethyl ) benzaldehyde, 3.3 g of methyl thioglycolate, 4.0 g of potassium carbonate and 50 ml of DMF was stirred at 60C for 2 hours, and then the reaction mixture was cooled to room temperature. To the reaction mixture was added water, and extracted with tert-butyl methyl ether 3 times. The combined organic layer was washed with water, followed by saturated aqueous sodium chloride solution. The mixture was dried over magnesium sulfate, and then concentrated under reduced pressure. The residue was recrystallized from methanol to obtain 6.3 g of methyl 5- (trifluoromethyl ) benzo[ b] thiophene-2- carboxylate. | |
6.3 g | With potassium carbonate; In N,N-dimethyl-formamide; at 60℃; for 2h; | Production Example 1 A mixture of 5.0 g of 2-fluoro-5-(trifluoromethyl)benzaldehyde, 3.3 g of methyl thioglycolate, 4.0 g of potassium carbonate and 50 ml of DMF was stirred at 60 C. for 2 hours. The reaction mixture was cooled down to room temperature. To the reaction mixture was added water, and the mixture was extracted with tert-butyl methyl ether three times. The combined organic layers were washed with water and saturated saline, and dried over magnesium sulfate, then, concentrated under reduced pressure. The residue was recrystallized from methanol, to obtain 6.3 g of methyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate (present condensed ring compound 1). [Present Condensed Ring Compound 1] [0100] 1H-NMR (CDCl3) δ: 8.16 (s, 1H), 8.13 (s, 1H), 7.99 (d, J=8.7 Hz, 1H), 7.67 (d, J=8.7 Hz, 1H), 3.98 (s, 3H) |
6.3 g | With potassium carbonate; In N,N-dimethyl-formamide; at 60℃; for 2h; | A mixture of 5.0 g of 2-fluoro-5-(trifluoromethyl)benzaldehyde, 3.3 g of methyl thioglycolate, 4.0 g of potassium carbonate and 50 ml of DMF was stirred at 60 C. for 2 hours. The reaction mixture was cooled down to room temperature. To the reaction mixture was added water, and the mixture was extracted with tert-butyl methyl ether three times. The combined organic layers were washed with water and saturated saline, and dried over magnesium sulfate, then, concentrated under reduced pressure. The residue was recrystallized from methanol, to obtain 6.3 g of methyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate (present condensed ring compound 1). [Present Condensed Ring Compound 1]. 1H-NMR (CDCl3) δ: 8.16 (s, 1H), 8.13 (s, 1H), 7.99 (d, J=8.7 Hz, 1H), 7.67 (d, J=8.7 Hz, 1H), 3.98 (s, 3H) |
General procedure: To a solution of 15a-m in DMF, K2CO3 (25 mmol, 3.45 g) wasadded and the mixturewas stirred at room temperature for 30 min.Then 16 was added dropwise. The reactionwas allowed to warm to60 C and monitored by TLC. The reaction was poured into waterand the mixture was extracted with ethyl acetate three times. Thecombined extracts were dried, concentrated and purified to affordthe intermediate 17a-m. Intermediate AM4a-mwas prepared in a similar manner as thatfor intermediate AM1, using 17a-m instead of 9. |
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