HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
Tetrahydrofuran → (S)-3-(2-chloro-3-fluorobenzyl)-1-(5-(1,3-dioxoisoindolin-2-yl)-1-hydroxypentan-2-yl)-1-methylurea
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | Tetrahydrofuran | HCID 8028 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | (S)-2-(5-hydroxy-4-(methylamino)pentyl)isoindoline-1,3-dione | HCID 57947589 | — |
| Edukt | (2-Chloro-3-fluorophenyl)methanamine hydrochloride | HCID 66622557 | — |
| Produkt | (S)-3-(2-chloro-3-fluorobenzyl)-1-(5-(1,3-dioxoisoindolin-2-yl)-1-hydroxypentan-2-yl)-1-methylurea | HCID 57947359 | 47% |
Reaktionsschritte
To a solution of 4-nitrophenylchloroformate (460 mg, 2.29 mmol) in THF (20 mL) was added 2-chloro-3-fluorobenzylamine hydrochloride (626 mg, 2.29 mmol) and DIEA (0.76 mL, 4.58 mmol) and the mixture was stirred at RT until TLC showed complete consumption of 2-chloro-3-fluorobenzylamine. The mixture was then added into a solution of (S)-2-(5-hydroxy-4-(methylamino)pentyl)isoindoline-1,3-dione (500 mg, 1.91 mmol) in THF (10 mL). The mixture was stirred overnight, concentrated and purified on RP-HPLC using a mixture of acetonitrile and H2O to give (S)-3-(2-chloro-3-fluorobenzyl)-1-(5-(1,3-dioxoisoindolin-2-yl)-1-hydroxypentan-2-yl)-1-methylurea (401 mg, 47%). LRMS (M+H+) m/z 448.3.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US08088793B2 |
| Quelldatensatz | uspto-grants-2012_01 |
| ORD ID | ord-ce77f78f5ef44b46896807ec97909b01 |
| Quellennotiz | uspto-grants-2012_01 |