HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
1,4-Dibromo-2-nitrobenzene → HCID 62896872, Verbindung
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | 1,4-Dibromo-2-nitrobenzene | HCID 77004 | — |
| Edukt | Diisopropylethylamine | HCID 81531 | — |
| Edukt | 1-(Aminomethyl)cyclopentan-1-ol--hydrogen chloride (1/1) | HCID 21109693 | — |
| Lösungsmittel | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Produkt | HCID 62896872 | HCID 62896872 | 43% |
Reaktionsschritte
The mixture of 2,5-dibromonitrobenzene (Tokyo Kasei Kogyo Co., Ltd., 5.4 g, 19.2 mmol), 1-(aminomethyl)cyclopentanol hydrochloride (J. Med. Chem. 1981, 24, 12-16, 4.3 g, 28.4 mmol) and N,N-diisopropylethylamine (8.4 mL, 48.1 mmol) in 1-methyl-2-pyrrolidinone (32 mL) was microwaved for 30 min at 200° C. The reaction was quenched with water and extracted three times with ethyl acetate. The combined organic layers were dried over sodium sulfate and filtered. The filtrate was concentrated and the residue was purified by column chromatography on silica gel (hexane:ethyl acetate=5:1 as eluent) to afford the title compound (2.6 g, 43%) as an orange amorphous solid.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US07598393B2 |
| Quelldatensatz | uspto-grants-2009_10 |
| ORD ID | ord-42a2a21addcc496abd29a1388410969d |
| Quellennotiz | uspto-grants-2009_10 |