HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 44399584, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 69587003 | HCID 69587003 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 44399584 | HCID 44399584 | — |
Reaction Steps
To a stirring solution of 8a in dichloromethane (0.1 M) at 0° C. under nitrogen was added triethylamine (3.5 eq) and methanesulfonyl chloride (1.1 eq). The reaction was stirred at room temperature overnight. The reaction mixture was washed with saturated sodium bicarbonate (1×), brine (1×), dried over sodium sulfate, filtered, concentrated in vacuo and purified by flash chromatography using the ISCO (0-15% gradient methanol/dichloromethane) to afford the product. (41%) 1H NMR (400 MHz, CDCl3) δ 7.16-7.46 (m, 9H), 6.79 (m, 1H), 6.12 (m, 1H), 4.32 (m, 2H), 4.03 (m, 1H), 3.70 (m, 1H), 3.36-3.17 (m, 1H), 2.90 (s, 2H), 2.47-2.83 (m, 6H), 1.74 (m, 6H), 1.25 (m, 1H). Mass Spectral Analysis m/z=430.3 (M+H)+ tR=3.70 min (96%)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06992193B2 |
| Source dataset | uspto-grants-2006_01 |
| ORD ID | ord-76f5f76e397440128d5eb4e5e1e0cb7b |
| Source note | uspto-grants-2006_01 |