HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Ethyl Acetate → 2,4-Dichloro-5-isopropyl-6-(2,3,5-trimethyl-phenoxy)-pyrimidine
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | 2,3,5-Trimethylphenol | HCID 12769 | — |
| Edukt | Sodium hydride | HCID 24758 | — |
| Edukt | 2,4,6-Trichloro-5-isopropylpyrimidine | HCID 249009 | — |
| Lösungsmittel | Dimethylformamide | HCID 6228 | — |
| Produkt | 2,4-Dichloro-5-isopropyl-6-(2,3,5-trimethyl-phenoxy)-pyrimidine | HCID 59184665 | 94% |
Reaktionsschritte
Sodium hydride (60%, 59 mg, 1.44 mmol. 1.1 eq.) was added to 2,3,5-trimethyl-phenol (179 mg, 1.31 mmol) in DMF (2 mL). The mixture was stirred at room temperature for 15 minutes and then added to 2,4,6-trichloro-5-isopropyl-pyrimidine (296 mg, 1.31 mmol) in 1 mL DMF. The reaction was stirred at room temperature for 4 hours. Ethyl acetate was added and washed with brine. The organic layer was concentrated down and purified (silica gel, 0-50% EtOAC/hexane) to give white solid (400 mg, 94%). LC-MS shows 325.2 (M+1). 1H NMR (300 MHz, CDCl3): δ 6.94 (s, 1H), 6.63 (s, 1H), 3.61 (m, 1H), 2.32 (s, 6H), 2.02 (s, 3H), 1.42 (d, 6H).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08106064B2 |
| Quelldatensatz | uspto-grants-2012_01 |
| ORD ID | ord-0e9d5a4705a9406daa7455443cbe0902 |
| Quellennotiz | uspto-grants-2012_01 |