Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Methanesulfonyl chloride | HCID 31297 | — |
| Reactant | HCID 18996959 | HCID 18996959 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 10067138 | HCID 10067138 | — |
Reaction Steps
2-Amino-9,10-dihydro-4,5-dimethoxy-9,10-dioxoanthracene (1.5 g) was dissolved in dry pyridine (30 ml) and freshly distilled methanesulphonyl chloride (0.61 g) slowly added. The mixture was heated to 90° C. for 3 hours under an atmosphere of nitrogen before being allowed to cool to room temperature. The mixture was then poured into water (150 ml), generating a brown precipitate. The solid was collected by filtration and dried in vacuo over silica gel to yield N-(4,5-dimethoxy-9,10-dihydro-9,10-dioxoanthracen-2-yl)methanesulphonamide at 94% purity (HPLC) as brown lustrous crystals. To improve purity, the crystals were dissolved in 2N sodium hydroxide solution, washed with CHCl3, and filtered to remove any remaining solid residue.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US05480873 |
|---|
| Source dataset | uspto-grants-1996_01 |
|---|
| ORD ID | ord-f391a51001e548348a208676f1b2b23c |
|---|
| Source note | uspto-grants-1996_01 |
|---|