HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 44581704, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 44581664 | HCID 44581664 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 44581704 | HCID 44581704 | — |
Reaction Steps
The product from Example 144 (0.017 g, 0.034 mmol) from was dissolved in CH2Cl2 (0.3 mL). Et3N (0.1 mL, 0.07 mmol) and MsCl (0.07 mL, 0.09 mmol) were added at rt under N2. The reaction was stirred for 12 h, concentrated to dryness, and purified via flash chromatography (silica, 100% EtOAc then 0.5% Et3N:10% MeOH:CH2Cl2) to afford the title compound. LC/MS (ESI+) 574.4 (M+H)+, tR=2.84 min (10–90% CH3CN/H2O in a 4-min run). 1H NMR ((CD3)2CO, 300 MHz) δ 7.50 (d, J=9.1 Hz, 2H), 7.33 (m, 4H), 6.98 (d, J=9.1 Hz, 2H), 4.16 (t, J=6.6 Hz, 2H), 3.83 (m, 7H), 3.16 (t, J=6.4 Hz, 2H), 2.42 (s, 3H), 1.47 (m, 2H), 1.18 (m, 2H) ppm.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07312214B2 |
| Source dataset | uspto-grants-2007_12 |
| ORD ID | ord-faacf4821c1c4256b4cb63fecf5c75c8 |
| Source note | uspto-grants-2007_12 |