HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 58764251, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | 2460749-55-5 | HCID 58764180 | — |
| Solvent | Hydrochloric Acid | HCID 313 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58764251 | HCID 58764251 | 57% |
Reaction Steps
To 1-(4-bromo-2-fluoro-phenyl)-1-methyl-ethylamine(1.2 g, 5.4 mmol) and triethylamine (900 μL, 6.5 mmol) in dichloromethane (10 mL) at room temperature was added methanesulfonyl chloride (500 μL, 6.5 mmol). The solution was stirred 16 h, diluted in 1N HCl(aq) and extracted with ethyl acetate. The organic layer was washed with saturated sodium bicarbonate, then saturated sodium chloride, dried (Na2SO4), filtered, and concentrated in vacuo to an off-white solid. Flash chromatography (SiO2, 40% ethyl acetate/hexane) gave a white solid (950 mg, 57%). 1H NMR (300 MHz, CDCl3): δ ppm 1.76 (s, 6 H) 2.74 (s, 3 H) 4.88 (s, 1 H) 7.24 (d, J=1.51 Hz, 1 H) 7.27–7.30 (m, 2 H)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07151105B2 |
| Source dataset | uspto-grants-2006_12 |
| ORD ID | ord-772b0ac519674b738b49f71672cb7eb8 |
| Source note | uspto-grants-2006_12 |