HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methane → HCID 178441331, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methane | HCID 297 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 178441330 | HCID 178441330 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 178441331 | HCID 178441331 | 195.6% |
Reaction Steps
To a solution of Example 61A (300 mg, 0.768 mmol) and triethylamine (233 mg, 2.305 mmol) in Et2O (5 mL) was added activated charcoal (10 mg, 0.768 mmol), followed by addition of bis(trichloromethyl) carbonate (114 mg, 0.384 mmol) and the mixture was stirred for 2 hr. The reaction was filtered, and concentrated to give the title compound as an oil (340 mg, 0.751 mmol, 98%). 1H NMR (300 MHz, DMSO-d6) δ ppm 1.33 (s, 9H) 3.80 (t, J=5.43 Hz, 2H) 4.27 (t, J=5.43 Hz, 2H) 7.32 (s, 1H) 7.46-7.56 (m, 1H) 7.88-7.97 (m, 1H) 8.24-8.33 (m, 1H); MS (DCI) m/z 453 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08058293B2 |
| Source dataset | uspto-grants-2011_11 |
| ORD ID | ord-caaa15e452304a80adf43e0f0374b093 |
| Source note | uspto-grants-2011_11 |