HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Water → 3-chloro-2-(4-(6-fluoropyridin-2-yl)benzyl)-7-isobutyl-5-methyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Water | HCID 962 | — |
| Edukt | Hexachloroethane | HCID 6214 | — |
| Edukt | Lithium Hexamethyldisilazide | HCID 2733832 | — |
| Edukt | 2-(4-(6-fluoropyridin-2-yl)benzyl)-7-isobutyl-5-methyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione | HCID 70094720 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Lösungsmittel | Tetrahydrofuran | HCID 8028 | — |
| Produkt | 3-chloro-2-(4-(6-fluoropyridin-2-yl)benzyl)-7-isobutyl-5-methyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione | HCID 70094773 | 107% |
Reaktionsschritte
2-(4-(6-fluoropyridin-2-yl)benzyl)-7-isobutyl-5-methyl-2H-pyrazolo[3,4-d]pyrimidine-4,6(5H,7H)-dione (450 mg, 1.1 mmol) and hexachloroethane (523 mg, 2.2 mmol) are dissolved in 5 mL of methylene chloride, and then 1.0 M LiHMDS (2.2 mL, 2.2 mmol) in THF is added dropwise. After the reaction mixture is stirred at room temperature for 10 min, water is added, and then extracted with methylene chloride three times. The combined organic phase is evaporated to dryness to give 520 mg of crude product as off-white solids, which is used in the next step without further purification. MS (ESI) m/z 442.2 [M+H]+.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US09434730B2 |
| Quelldatensatz | uspto-grants-2016_09 |
| ORD ID | ord-44f8ed79dd3b4c0d9f60cc731de38f25 |
| Quellennotiz | uspto-grants-2016_09 |