HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chlorosuccinimide → 3-butyl-8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | 3-butyl-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione | HCID 59299589 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 3-butyl-8-chloro-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione | HCID 59299582 | 64% |
Reaction Steps
To a solution of 3-butyl-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (3.34 g, 13.4 mmol) in anhydrous DMF (19 ml) was added NCS (1.97 g, 14.8 mmol) and left to stir at rt under nitrogen for 22 hours. The mixture was concentrated in vacuo to give a yellow solid which was filtered and washed with methanol. The filtrate was concentrated and the process repeated. On the final wash the filtrate was purified by SPE (Si, 20 g) cartridge eluting with 1:1; EtOAc:cyclohexane. The combined solids were dried under vacuum to afford the title compound (2.42 g, 64%); m/z 283.3 [MH+]
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08268839B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-d556e82ec3044461969e66f9c2e3f1f6 |
| Source note | uspto-grants-2012_09 |