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CAS No. : | 393-53-3 | MDL No. : | MFCD03789251 |
Formula : | C6H4FNO2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | POLXLLIQWDBJMD-UHFFFAOYSA-N |
M.W : | 141.10 | Pubchem ID : | 345361 |
Synonyms : |
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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 |
---|---|---|
24% | Example 117: 3-l(3-thienylmethyl)aminol-4-pyridinecarboxylic acid hydrochloride To a mixture of 3-fluoro-4-pyridinecarboxylic acid (200 mg, 1.417 mmol) and N-ethyl-N-(1-methylethyl)-2-propanamine (619 p1, 3.54 mmol) was added <strong>[27757-86-4](3-thienylmethyl)amine</strong> (198 mg, 1 .701mmol). The reaction mixture was heated using a microwave 160C for 4hr then diluted with DMSO (4ml) and purified by MDAP (High pH modifier, Method E) to give the free base compound as a whitesolid (83 mg). This was dissolved in 1 ,4-Dioxane (3 ml) then 2N HCI in ether (178 p1, 0.356 mmol)was added and the resulting solution concentrated under reduced pressure to give the title compoundas a yellow solid (92 mg, 24%)LCMS (Method B): Rt = 0.55 mins, MH+ = 235.1 |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
93% | In 1,4-dioxane; water; at 140℃; for 14.0h; | 3-Fluoroisonicotinic acid (3.00 g, 21.3 mmol) was dissolved in dioxane (6 mL) and 30% aqueous methylamine solution (22.0 g, 213 mmol) was added. The reaction solution was heated to 140C and stirred for 14 hours. Conc. hydrochloric acid (12 N, 3 mL) was added and the pH was adjusted to 3, filtered and the filter cake was dried to give 3-(methylamino)isonicotinic acid (3.00 g, as a yellow solid) with a yield of 93%. 1H NMR: (400 MHz, DMSO-d6) delta 8.46(br, 1H), 7.89(s, 1H), 7.69(d, J = 5.2 Hz, 1H), 7.50(d, J = 5.2 Hz, 1H), 2.80(s, 3H). |
93% | In 1,4-dioxane; water; at 140℃; for 14.0h; | 3-Fluoroisonicotinic acid (3.00 g, 21.3 mmol) was dissolved in dioxane (6 mL), and then 30% methylamine aqueous solution (22.0 g, 213 mmol) was added. The reaction solution was heated to 140 C. and then stirred for 14 hours. Concentrated hydrochloric acid (12N, 3 mL) was added to adjust the pH value to pH=3, followed by filtration. The filter cake was dried to give 3-(methylamino)isonicotinic acid (3.00 g, yellow solid) with a yield of 93%. 1H NMR: (400 MHz, DMSO-d6) delta8.46 (s, 1H), 7.89 (s, 1H), 7.69 (d, J=4.8 Hz, 1H), 7.50 (d, J=4.8 Hz, 1H), 2.80 (s, 3H). |
42% | In 1,4-dioxane; water; at 125℃; for 9.5h;Microwave irradiation; | Example 153: 3-(methylamino)-4-pyridinecarboxylic acid Methylamine (0.321 mL,3.90 mmol, 40% solution in water) was added to a 3-fluoro-4- pyridinecarboxylic acid (250 mg, 1 .772 mmol) and 1 ,4-Dioxane (0.3 ml) and the mixture heated using a microwave to 125 C for 1.5 hr then 2 hr and finally an additional 6 hr. The mixture was allowed tocoolthen concentrated by evaporation. Water (10 ml) was added then the mixture acidifed to pH 3 using 37% HCI. The resulting bright yellow precipitate was filtered then washed with water (10 ml) to give the title compound as a yellow solid, 114 mg (42%).1H NMR (400 MHz, DMSO-S6) 8.2oppm (1H, 5), 7.84ppm (1H, d), 7.Ssppm (1H, d), 2.93ppm (3H, 5). |
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