HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hexane → 1245830-98-1
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hexane | HCID 8058 | — |
| Reactant | 2,4,5-Trichloropyrimidine | HCID 237259 | — |
| Reactant | Sodium methanethiolate | HCID 4378561 | — |
| Solvent | Iodine | HCID 807 | — |
| Solvent | Oxolane--water (1/1) | HCID 21881883 | — |
| Product | 1245830-98-1 | HCID 58200927 | 94.8% |
Reaction Steps
To a solution of 2,4,5-trichloropyrimidine (5 g, 27.32 mmol) in THF:water (1:1, 40 mL), was added sodium thiomethoxide (2.15 g, 30.01 mmol) at 0° C., and the mixture was stirred at rt for 4 h. TLC showed completion of starting material and formation of a slightly polar spot (TLC system: hexane charred in iodine). The reaction mixture was concentrated, water (20 ml) was added, and the product was extracted with ethyl acetate (2×20 ml). The organic layer was dried over sodium sulfate and concentrated to afford the desired compound as a white solid (5 g, 94.8%). MS m/z: 195.2 (ES+, M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09145387B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-104623fcea224ed6af37325f88f6954c |
| Source note | uspto-grants-2015_09 |