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CAS No. : | 1017779-51-9 | MDL No. : | MFCD09258697 |
Formula : | C9H9BrF2O | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 251.07 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Danger | Class: | 8 |
Precautionary Statements: | P260-P264-P270-P280-P301+P330+P331-P303+P361+P353-P304+P340-P305+P351+P338-P310-P363-P405-P501 | UN#: | 3261 |
Hazard Statements: | H302-H314 | Packing Group: | Ⅱ |
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 carbon tetrabromide; triphenylphosphine In dichloromethane at 20℃; |
Yield | Reaction Conditions | Operation in experiment |
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With potassium carbonate In acetonitrile Reflux; |
Yield | Reaction Conditions | Operation in experiment |
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14% | With caesium carbonate In N,N-dimethyl-formamide at 20℃; Inert atmosphere; | ntermedate 1-1-1Preparation of 1-(4-ethoxy-2,6-dfluorobenzy-1 ,4,5,6-tetrahydrocycopenta[c]- pyrazoe-3-carbonftrHe ntermedate 1-1-1Preparation of 1-(4-ethoxy-2,6-dfluorobenzy-1 ,4,5,6-tetrahydrocycopenta[c]- pyrazoe-3-carbonftrHe3.40 g of I ,4,5,6-tetrahydrocycopenta[c]pyrazoe-3-carbonftrHe (CAS-RN851776-29-9) (25.5 mmo, 1.00 eq.) were dssoved n 35 mL dry DMF under n[trogen atmosphere. 7.05 g 2-(bromomethy-5-ethoxy-1 ,3-dfluorobenzene(28.1 mmo, 1.10 eq.) and 9.98 g cesumcarbonate (30.1 mmo, 1.20 eq.) were added and stirred over nght at rt. DCM and water were added, the aqueous phase was washed twice wfth DCM, the organic phase was washed wth brine and was dried w[lh magnesumsufate, was concentrated n vacuo and purified by flash chromatography (hexanel tert-buty methy ether gradent w[th hexane100-70%) to provde 1.07 g (3.45 mmo, 14 %) of the anaytcaHy pure target compound.1H-NMR (300MHz, DMSO-d6): ö [ppm]= 1 .27 (t, 3H), 2.11 2.23 (m, I H), 2.38 -2.45 (m, I H), 2.54 - 2.68 (m, 4H), 4.02 (q, 2H), 5.22 (s, 2H), 6.71 6.79 (d, 2H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
85% | 185 g of <strong>[43120-28-1]methyl 1H-indazole-3-carboxylate</strong> (1 050 mmol, 1 .0 eq.) were dissolved in3 L of dry THF and cooled to 5 C. 411 g of cesium carbonate (1260 mmol, 1.2 eq.) were added stirred for 15 mm. 290 g of 2-(bromomethyl)-5-ethoxy-1,3-difluorobenzene (1155 mmol, 1.1 eq.) dissolved in 250 mL THF were added drop wise at 5 C. The precipitate was filtered off. The filtrate was concentrated in vacuo. The residue was crystallized from ethyl acetate/hexane (1:1) to provide 310 g (895 mmol, 85 %) of analytically pure target compound. 1H NMR (400 MHz, DMSO-d6) delta [ppm]= 1.27 (t, 3H), 3.86 (s, 3H), 4.01 (q, 2H),5.68 (s, 2H), 6.70-6.76 (m, 2H), 7.32 (t, 1H), 7.50 (t, 1H), 7.84 (d, 1H), 8.00-8.12(m, 1H). | |
85% | Intermediate 1-7-1Preparation of methyl 1 -(4-ethoxy-2,6-difluorobenzyl)-1 H-indazole-3-carboxylate185 g of methyl 1 H-indazole-3-carboxylate (1050 mmol, 1.0 eq.) were dissolved in 3 L of dry THF and cooled to 5 . 41 1 g of cesium carb onate (1260 mmol, 1 .2 eq.) were added stirred for 15 min. 290 g of 2-(bromomethyl)-5-ethoxy-1 ,3-difluorobenzene (1 155 mmol, 1 .1 eq.) dissolved in 250 ml THF were added drop wise at 5 . The precipitate was filtered off. The filtrate was concentrated in vacuo. The residue was crystallized from ethyl acetate/hexane (1 :1 ) to provide 310 g (895 mmol, 85 %) of analytically pure target compound.1H-NMR (400 MHz, DMSO-d6) delta [ppm]= 1 .27 (t, 3H), 3.86 (s, 3H), 4.01 (q, 2H), 5.68 (s, 2H), 6.70 - 6.76 (m, 2H), 7.32 (t, 1 H), 7.50 (t, 1 H), 7.84 (d, 1 H), 8.00 - 8.12 (m, 1 H). | |
85% | 185 g of methyl 1 H-indazole-3-carboxylate (1050 mmol, 1 .0 eq.) were dissolved in 3 I of dry THE and cooled to 5 C. 411 g of caesium carbonate (1260 mmol, 1.2 eq.) were added stirred for 15mm 290 g of 2-(bromomethyl)-5-ethoxy-1,3-difluorobenzene (1155 mmol, 1 .1 eq.) dissolved in 250 ml THE were added drop wise at 5 C. The precipitatewas filtered off. The filtrate was concentrated in vacuo. The residue was crystallized from Ethyl acetate/Hexane (1:1) to provide 310 g (895 mmol, 85 %) of analytically puretarget compound.1H NMR (400 MHz, DMSO-d6) 6 [ppm]= 1.27 (t, 3H), 3.86 (5, 3H), 4.01 (q, 2H), 5.68 (5,2H), 6.70-6.76 (m, 2H), 7.32 (t, 1H), 7.50 (t, 1H), 7.84 (d, 1H), 8.00-8.12 (m, 1H). |
85% | 185 g of <strong>[43120-28-1]methyl 1H-indazole-3-carboxylate</strong> (1050 mmol, 1.0 eq.) were dissolved in 3 I ofdry THE and cooled to 5 C. 411 g of cesium carbonate (1260 mmol, 1 .2 eq.) were addedstirred for 15 mm. 290 g of 2-(bromomethyl)-5-ethoxy-1,3-difluorobenzene (1155 mmol,1 .1 eq.) dissolved in 250 ml THE were added drop wise at 5 C. The precipitate wasfiltered off. The filtrate was concentrated in vacuo. The residue was crystallized from EE /hexane (1:1) to provide 310 g (895 mmol, 85%) of analytically pure target compound.1H NMR (400 MHz, DMSO-d6) 6 [ppm]= 1.27 (t, 3H), 3.86 (5, 3H), 4.01 (q, 2H), 5.68 (5, 2H), 6.70-6.76 (m, 2H), 7.32 (t, 1H), 7.50 (t, 1H), 7.84 (d, 1H), 8.00-8.12 (m, 1H). | |
21.18 g | With caesium carbonate; In tetrahydrofuran; at 0 - 20℃; for 5h;Inert atmosphere; | 9.98 g of methyl 1 H-indazole-3-carboxylate (56.65 mmol, 1 eq.) were dissolved in 260 ml_ of dry tetrahydrofuran at 0C. 22.15 g of ce sium carbonate (67.98 mmol, 1.2 eq.) and 15.65 g 2-(bromomethyl)-1 ,3-difluorobenze (62.31 mmol, 1.1 eq.) were added. The mixture was stirred at room temperature for five hours under nitrogen atmosphere. Then the reaction mixture was concentrated in vacuo. The residue was partitioned between dichloromethane and half saturated aqueous sodium bicarbonate solution. The organic layer was washed with water, dried over sodium sulfate and concentrated in vacuo yielding 21 .18 g of the titel compound (61 .15 mmol, 108.0%). The material was pure enough for further processings. H NMR (400 MHz, DMSO-d6) delta [ppm]= 1.26 (t, 3H), 3.86 (s, 3H), 4.01 (q, 2H), 5.68 (s, 2H), 6.73 ("d", 2H), 7.33 ("t", 1 H), 7.51 ("t", 1 H), 7.83 ("d", 1 H), 8.04 ("d", 1 H). LC-MS: retention time: 1 .34 min (method 1 ) MS ES+: 347.1 [M+H]+ |