HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine hydrochloride → 2,4-Dichloro-5-phenylpyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine hydrochloride | HCID 11130 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | 5-Phenyluracil | HCID 287110 | — |
| Product | 2,4-Dichloro-5-phenylpyrimidine | HCID 12356597 | 100% |
Reaction Steps
To 5-Phenyl-1H-pyrimidine-2,4-dione (110 mg, 0.585 mmol) and triethyl amine hydrochloride (317 mg, 2.3 mmol) was added POCl3 (15 mL) and the solution was heated to 120 C for 72 h. POCl3 was removed in vacuum and the resulting brown oil was quenched with ice water and treated with saturated NaHCO3, extracted with ethyl acetate, washed with brine, dried (Na2SO4) to give 2,4-Dichloro-5-phenyl-pyrimidine 131 mg (100% yield). HPLC tr=7.09 min (100%), FIA-MS 224.9 (M+H), HNMR (500 MHz, CDCl3) 8.49 (1H, s), 7.45 (3H, m), 7.35 (2H, m).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07842712B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-883b35b8669b4d9597e9c1296fff4e56 |
| Source note | uspto-grants-2010_11 |