HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 68681999, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | 4-Bromo-2-fluorobenzene-1-sulfonyl chloride | HCID 2736310 | — |
| Reactant | HCID 58988130 | HCID 58988130 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68681999 | HCID 68681999 | 38.8% |
Reaction Steps
6-[(3R,5S)-3,5-Dimethyl-1-piperazinyl]-3-(methyloxy)-2-pyridinamine (D7, Method D) (2.25 mmol) was dissolved in DCM (5 mL) and pyridine (5 mL) and then cooled to 0° C. 4-Bromo-2-fluoro benzenesulfonyl chloride (0.738 g, 2.706 mmol), dissolved in DCM (5 mL) was then added dropwise and the reaction then allowed to warm to rt overnight. The reaction was then evaporated to a minimum and redissolved in DCM (100 mL) and washed with water (2×75 mL), saturated sodium hydrogen carbonate (3×75 mL) and brine (75 mL). The organic layer was dried (MgSO4) and evaporated to give a brown oil which was triturated with methanol and dried at 50° C. under high vac to give the title compound as a pale brown powder (D18) (0.400 g). MS (ES+) m/e 473/475 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07713978B2 |
| Source dataset | uspto-grants-2010_05 |
| ORD ID | ord-d7df2eebecd34a919d8b762be15a45ff |
| Source note | uspto-grants-2010_05 |