HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Triethylamine → 4-(4-Fluoro-3-isocyanato-benzyl)-2H-phthalazin-1-one
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Triethylamine | HCID 8471 | — |
| Edukt | Triphosgene | HCID 94429 | — |
| Edukt | 4-(3-amino-4-fluorobenzyl)-2H-phthalazin-1-one | HCID 18444373 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 4-(4-Fluoro-3-isocyanato-benzyl)-2H-phthalazin-1-one | HCID 59856545 | — |
Reaktionsschritte
To a suspension of 4-(3-amino-4-fluoro-benzyl)-2H-phthalazin-1-one (1)(4.0 g, 14.8 mmol) in anhydrous DCM (1.6 L) and triethylamine (4.62 mL, 40.86 mmol), was added a dropwise preformed solution of triphosgene (2.75 g, 9.28 mmol) in anhydrous DCM (327 mL) and stirred for 70 minutes and room temperature. The reaction mixture was then concentrated to dryness in vacuo yielding a grey solid. Single peak in LC-MS analysis, (yield taken to be quantitative) no purification performed. m/z (LC-MS, ESP), RT=4.49 mins, (M+MeOH) 328.0.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07902193B2 |
| Quelldatensatz | uspto-grants-2011_03 |
| ORD ID | ord-78509e2f26d7418f81df896423ac6f67 |
| Quellennotiz | uspto-grants-2011_03 |