HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-methyl-2-pyrrolidone → 2,2'-(Disulphanediyldiethane-2,1-diyl)bis(6-chloro-1H-benzo[de]-isoquinoline-1,3(2H)-dione)
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Reactant | 1H,3H-Naphtho[1,8-cd]pyran-1,3-dione, 6-chloro- | HCID 77672 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2-[(2-Aminoethyl)disulfanyl]ethan-1-amine hydrochloride | HCID 167628 | — |
| Product | 2,2'-(Disulphanediyldiethane-2,1-diyl)bis(6-chloro-1H-benzo[de]-isoquinoline-1,3(2H)-dione) | HCID 59428884 | — |
Reaction Conditions
| Temperature | 120 °C |
|---|
Reaction Steps
9.30 g of 6-chloro-1H,3H-benzo[de]isochromene-1 ,3-dione and 4.46 g of hydrochlorided cystamine hydrochloride are suspended in 50 ml of N-methylpyrrolidone (NMP). 5.5 g of diisopropylethylamine are added and the mixture is heated with stirring at 120° C. After two hours, 50 ml of NMP are added and the mixture is kept with stirring at 120° C. for 3 hours. After cooling, the precipitated product is recovered and the filtered solution is extended by addition of 200 ml of water, and a second precipitate is recovered. The precipitates are washed with water and dried. 11.46 g of white powder are recovered. The analyses show that the product is in accordance with the expected product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08038731B2 |
| Source dataset | uspto-grants-2011_10 |
| ORD ID | ord-ee6a623d63a74f3484eefa9efffc054f |
| Source note | uspto-grants-2011_10 |