HuagongsheHuagongshe Chemistry Print Report · For research reference only
Phosphorus oxychloride → HCID 59299534, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 59299542 | HCID 59299542 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59299534 | HCID 59299534 | 109.7% |
Reaction Steps
A solution of 1,3-dibutyl-2,6-dioxo-7-(2-propen-1-yl)-2,3,6,7-tetrahydro-1H-purine-8-carboxamide (300 mg) in anhydrous DMF (7 ml) at 0° C. was treated dropwise with POCl3 (237 uL). The ice-bath was removed and after 2 hours the mixture was partitioned between water and Et2O. The aqueous layer was re-extracted with Et2O and the combined extracts separated, washed with water (×2), brine, then dried (MgSO4) and concentrated, giving a yellow oil (312 mg). The oil was taken up in cyclohexane and purified by SPE (Si, 10 g) eluting with EtOAc/cyclohexane mixtures. Concentration of the product fractions gave the title compound as a colourless oil (150 mg, 53%); m/z. 330.3 [MH+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08268839B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-527d7cfa752b45edaf4846c5c58b97dc |
| Source note | uspto-grants-2012_09 |