HuagongsheHuagongshe Chemie-Druckbericht · Nur für Forschungszwecke
N-methylhydroxylamine hydrochloride → 3-(N-methyl-hydroxycarbamoyl)-5-nitro-benzoic acid allyl ester
Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|---|---|---|
| Edukt | N-methylhydroxylamine hydrochloride | HCID 77906 | — |
| Edukt | 5-Nitro-isophthalic acid 1-(2,5-dioxo-pyrrolidin-1-yl) ester 3-allyl ester | HCID 22986099 | — |
| Lösungsmittel | Dichloromethane | HCID 6344 | — |
| Produkt | 3-(N-methyl-hydroxycarbamoyl)-5-nitro-benzoic acid allyl ester | HCID 22986101 | 88,9% |
Reaktionsschritte
Starting material (8(c)) was prepared as follows. A mixture of 7(b) (2.00 g; see Example 7), N-methylhydroxylamine hydrochloride (1.06 g) triethylamine (1.72 ml) and dichloromethane (60 ml.) was stirred at 5° or 30 minutes. It was then allowed to warm to ambient temperature and stirred for a further 16 hours. The reaction mixture was then poured directly onto a flash column eluting with ethyl acetate/hexane (50:50) to give 3-(N-methyl-hydroxycarbamoyl)-5-nitro-benzoic acid allyl ester (8(a)) as a cream solid (1.43 g).
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patentnummer | US06232338B1 |
| Quelldatensatz | uspto-grants-2001_05 |
| ORD ID | ord-8eaf5aa4cfe0494f8a6de93fa605939b |
| Quellennotiz | uspto-grants-2001_05 |