HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 24960299, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1,1'-Carbonyldiimidazole | HCID 68263 | — |
| Reactant | Methanesulfonamide | HCID 72879 | — |
| Reactant | HCID 24959564 | HCID 24959564 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 24960299 | HCID 24960299 | 95.3% |
Reaction Steps
To a solution of 3 (0.5 g, 1.6 mmol) in dry CH2Cl2 (10 ml), N,N-carbonyldiimidazole (0.33 g, 2.0 mmol) was added under vigorous stirring. After 1 h methanesulfonamide (0.19 g, 2 mmol) and triethylamine (0.28 mL, 2 mmol) were added and the resulting mixture was left stirring overnight at room temperature. The organic mixture was washed with a saturated solution of NaHCO3 (2×10 mL) and brine (3×10 mL), dried over Na2SO4 and evaporated under vacuum to give pure 17 as a colourless oil (0.60 g, yield 95%). [α]b=+9 (c=1; CH3OH). 1H-NMR (DMSO-d6) δ 7.70 (d, 2H, J=7 Hz), 7.55 (d, 2H, J=7 Hz), 3.05 (s, 3H), 1.85 (d, 3H, J=23 Hz).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08440711B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-9e765c85c754413081ff83b1284ebfba |
| Source note | uspto-grants-2013_05 |