HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methoxybenzenesulfonyl chloride → HCID 22482377, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methoxybenzenesulfonyl chloride | HCID 7401 | — |
| Reactant | HCID 22482300 | HCID 22482300 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 22482377 | HCID 22482377 | 87% |
Reaction Steps
A solution of 6-ethyl-5,6-dihydrophenanthridine (14 g, 69.2 mmol) and 4-methoxybenzenesulfonyl chloride (17.2 g, 83 mmol) in pyridine (100 ml) was heated at 80° C. overnight. The solvent was evaporated in vacuo; and the crude product was purified by preparative column chromatography on silica gel, eluting with a gradient and mixture of dichloromethane-hexane (50:50 to 100:0). After evaporation of the solvent, the residue was crystallized from diethyl ether, yielding the title compound (22.8 g, 60.1 mmol, 87%) as a colorless, crystalline solid, which was characterized by LCMS (ES+, FA, CV=5) and 1H NMR.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06894061B2 |
| Source dataset | uspto-grants-2005_05 |
| ORD ID | ord-be6c317a515148e1a3b02c7fc72589f8 |
| Source note | uspto-grants-2005_05 |