HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 58994166, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | 1-Bromo-3-chloropropane | HCID 8006 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | O,O'-Bis(trimethylsilyl)-5-fluorouracil | HCID 140203 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 58994166 | HCID 58994166 | — |
Reaction Steps
A mixture of 5-fluoro-2,4-bis[(trimethylsilyl)oxy]pyrimidine (1 g, commercially available from Lancaster), 1-bromo-3-chloropropane (0.44 mL) and I2 (10 mg) in 1,2-dichloroethane (10 mL) was heated to reflux for 30 h. Then the reaction mixture was treated with water and the pH was brought to 7 using aqueous 6N NaOH solution, the mixture was extracted twice with DCM, the organic phase dried over Na2SO4 and the solvent evaporated under reduced pressure. The crude product was purified by flash chromatography on silica gel eluting with DCM/MeOH 95/5 to give 35 mg of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07727988B2 |
| Source dataset | uspto-grants-2010_06 |
| ORD ID | ord-0f56a0657d244ad79378abcbc156cbfa |
| Source note | uspto-grants-2010_06 |