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CAS No. : | 154350-29-5 | MDL No. : | MFCD08705286 |
Formula : | C3H7NO2S | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | WMSPXQIQBQAWLL-UHFFFAOYSA-N |
M.W : | 121.16 | Pubchem ID : | 15765418 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H332-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 |
---|---|---|
71% | The title compound from Example 2 (21.0 mg, 0.031 mmol) and carbonyldiimidazole (6.0 mg, 0.037 mmol) were dissolved in 0.7 ml anhydrous DMF and the resulting solution was heated to 40 C. for 1 hour. Cyclopropylsulfonamide (8.0 mg, 0.06 mmol) was added to the reaction followed by DBU (7.0 mg, 0.046 mmol). The reaction mixture was stirred at 40 C. for 10 hour. LCMS showed the formation of the desired product. The reaction was cooled down and 10 ml ethyl acetate was added to the solution. The mixture was washed with saturated aqueous NaHCO3 solution, water and brine. The organic layer was dried over anhydrous sodium sulfate. The organic phase was then filtered, concentrated in vacuo and subsequently purified by flash chromatography (ethyl acetate/hexanes 1:1) to give 17.0 mg (71%) of the title compound. MS (ESI) m/z 779.2 (M+H)+. 1H-NMR (500 MHz, CD3Cl): δ 10.24 (1H, s), 8.10 (1H, s), 8.00 (1H, d, J=8.0 Hz), 7.82 (1H, d, J=8.0 Hz), 7.60 (2H, m), 7.49 (1H, d, J=5.0 Hz), 7.16 (1H, s), 6.91 (1H, s), 6.09 (1H, s), 5.67 (1H, m), 5.12 (1H, m), 4.98 (1H, t, J=8.0 Hz), 4.70 (1H, t, J=8.0 Hz), 4.62 (2H, s), 4.33 (1H, m), 4.10 (1H, m), 2.92 (1H, m), 2.75 (2H, m), 2.58 (2H, m), 2.28 (1H, m), 1.91 (2H, m), 1.60-0.80 (20H, m). 13C-NMR (125 MHz, CD3Cl, 200-40 ppm region): δ 177.1, 173.5, 168.1, 155.2, 152.5, 140.7, 139.8, 139.1, 136.5, 130.5, 130.4, 129.7, 128.7, 128.3, 127.6, 127.1, 124.8, 80.1, 75.8, 59.7, 53.5, 52.3, 44.8. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
48% | Example 1570 Compound 1570 A was prepared from Compound 400 and 4-iodobenzoic acid by sequential application of the procedures given in Parts H and I in Example 400. Solid carbonyl diimidazole (19 mg, 0.12 mmol) was added in one portion to a stirred solution of Compound 1570A in THF (200 mL). The solution was stirred at 70 0C for 1.5 h, and was subsequently allowed to cool to rt. Solid <strong>[154350-29-5]cyclopropanesulfonamide</strong> (17 mg, 0.14 mmol) and DBU (43 mL, 43 mg, 0.29 mmol) were added sequentially and the reaction mixture was stirred at rt for 18 h. The solvent was evaporated and the residue was dissolved in DCM (50 mL). The solution was washed sequentially with 0.1 N aq hydrochloric acid (~25 mL), water (~25 mL) and brine (~25 mL). The organic phase was dried over anhydrous MgSCM, filtered and concentrated under reduced pressure to afford an off-white solid. The crude product was purified by PTLC (3:1 EtOAc-hexanes + 1% HCO2H) to afford the desired Compound 1570 (24 mg, 48% yield) as a beige solid. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51% | The title compound from Example 2 (2c) (6.0 mg, 0.01 mmol) and carbonyldiimidazole (2.0 mg, 0.01 mmol) were dissolved in 0.75 ml anhydrous DMF and the resulting solution was heated to 40 0C for 1 h. Cyclopropylsulfonamide (3.6 mg, 0.03 mmol) was added to the reaction followed by DBU (4.5 mg, 0.03 mmol). The reaction mixture was stirred at 40 0C, until completion was confirmed by MS analysis. The reaction was diluted with 10 ml ethyl acetate and extracted with saturated aqueous with NaHCO3 (2 x 2 mL) and brine (1 x 2 mL). The organic phase was dried over anhydrous Na2SO4, filtered, and then concentrated in vacuo. The residue was purified by silica gel flash chromatography using gradient elution with MeOH in DCM (1%→2%→5%) affording affording pyridazinone 4a. (4.0 mg, 51 %) MS (ESI) m/z = 787.3 (M+H)+. |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
51% | The title compound from Example 2 (6.0 mg) and carbonyldiimidazole (2.0 mg) were dissolved in 0.75 ml anhydrous DMF and the resulting solution was heated to 40 0C for 1 h. Cyclopropylsulfonamide (3.6 mg) was added to the reaction followed by DBU (4.5 mg). The reaction mixture was stirred at 40 0C, until completion was confirmed by MS analysis. The reaction was diluted with 10 ml ethyl acetate and extracted with saturated aqueous with NaHCCh (2 x 2 mL) and brine (1 x 2 mL). The organic phase was dried over anhydrous Na2SO4, filtered, and then concentrated in vacuo. The residue was purified by silica gel flash chromatography using gradient elution with MeOH in DCM (1%- >2%- >5%) affording the title compound. (4.0 mg, 51 %) MS (ESI) m/z = 811.42 (M+H)+. |
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