HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 15307969, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Methyl-2-thenoyl Chloride | HCID 2737605 | — |
| Reactant | HCID 15410466 | HCID 15410466 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 15307969 | HCID 15307969 | 70.7% |
Reaction Steps
To 0.193 g (1.2 mmol) of 3-methylthiophene-2-carbonyl chloride in 3 ml of dichloromethane, cooled to 0° C., is added 209 μl of triethylamine. The mixture is stirred and 0.30 g (1 mmol) of 5-(4-aminobenzoyl)-5,6-dihydrophenanthridine is added. The mixture is stirred at room temperature overnight and then concentrated under vacuum. To the residue is added 30 ml of ethyl acetate and the mixture washed with 2 ml each of water, 2N citric acid, 1M sodium bicarbonate and brine. The organic layer is dried (Na2SO4) and the solvent removed to give 0.30 g of solid. The solid is chromatographed on thick layer silica gel plates with ethyl acetate-hexane (1:1) as solvent to give 150 mg of product as a yellow foam.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05760031 |
| Source dataset | uspto-grants-1998_06 |
| ORD ID | ord-c38dcccf8c3842bea57d12cf516dfe76 |
| Source note | uspto-grants-1998_06 |