HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 14276135, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 14720261 | HCID 14720261 | — |
| Reactant | HCID 136197565 | HCID 136197565 | — |
| Solvent | Hexamethylphosphoramide | HCID 12679 | — |
| Product | HCID 14276135 | HCID 14276135 | 93.4% |
Reaction Steps
In 10 ml of hexamethylphosphoric triamide were dissolved 1 g of 6-hydroxy-3-ethyl-5-methyl-2-methylthio-4(3H)-pyrimidinone and 1.66 g of 4-(4'-trifluoromethylphenoxy)benzyl bromide and thereto was added 0.3 g of sodium hydride (55% in mineral oil). The mixture was stirred for 15 hours at room temperature. The resulting solution was poured into 50 ml of water and then extracted twice with 30 ml of ethyl ether. The ethyl ether layer was washed with water, dried over anhydrous sodium sulfate and freed of solvent by distillation under reduced pressure to give 2.1 g of crystals. The crystals were recrystallized from a mixture of hexane and ethyl ether (3:1 ) to give 0.6 g of the intended product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04908379 |
| Source dataset | uspto-grants-1990_03 |
| ORD ID | ord-ac763ec1f86f4e37920518fd772594b7 |
| Source note | uspto-grants-1990_03 |