HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl Sulfate → HCID 20158316, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 14011782 | HCID 14011782 | — |
| Product | HCID 20158316 | HCID 20158316 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
4,6-Dimethyl-5-hydroxy-2-phenpentylaminopyrimidine (0.5 g, 1.8 mmol) prepared by the method of example 1 was dissovled in dry THF (20 ml) under nitrogen and treated with sodium hydride (0.07 g, 1.8 mmol, 60% oil dispersion). The reaction mixture was stirred at 0° C. for 2 hours. Dimethylsulfate (0.11 ml, 1.8 mmol) was added with a syringe and the reaction was stirred for an additional hour. After quenching with saturated NH4Cl (aqueous, 20 ml), the reaction mixture was extracted with ethylacetate (75 ml). The extracts were washed with 50 ml water and 50 ml brine, dried over MgSO4 and concentrated. Chromatography on silica gel with ethylacetate/hexane (1:1) eluent yielded 0.15 g of the title compound as a yellow oil, m.p.: 31° to 33° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04711888 |
| Source dataset | uspto-grants-1987_12 |
| ORD ID | ord-6d0a7362a81a4c54bf2315305fd02ba9 |
| Source note | uspto-grants-1987_12 |