Triethylamine → 3-(N-methyl-methoxycarbamoyl)-5-nitro benzoic acid allyl ester

HRID 1263604Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1263604
[CH2:1]([O:4][C:5](=[O:25])[C:6]1[CH:7]=[C:8]([CH:19]=[C:20]([N+:22]([O-:24])=[O:23])[CH:21]=1)[C:9]([O:11]N1C(=O)CCC1=O)=O)[CH:2]=[CH2:3].Cl.[CH3:27][NH:28][O:29][CH3:30].C(N(CC)CC)C>ClCCl>[CH2:1]([O:4][C:5](=[O:25])[C:6]1[CH:21]=[C:20]([N+:22]([O-:24])=[O:23])[CH:19]=[C:8]([C:9](=[O:11])[N:28]([O:29][CH3:30])[CH3:27])[CH:7]=1)[CH:2]=[CH2:3]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)HCID 229860995-Nitro-isophthalic acid 1-(2,5-dioxo-pyrrolidin-1-yl) ester 3-allyl ester

Produkt 1

HCID 206558613-(N-methyl-methoxycarbamoyl)-5-nitro benzoic acid allyl ester

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of (7(b)) (2.00 g), N,O-dimethylhydroxylamine hydrochloride (0.62 g), triethylamine (0.86 ml) and dichloromethane (60 ml) was stirred at 50 for 30 min and then allowed to warm to ambient temperature and stirred for a further 16 h. The mixture was poured onto a flash column and eluted with ethyl acetate/hexane (40:60) to give 3-(N-methyl-methoxycarbamoyl)-5-nitro benzoic acid allyl ester (7(c)) as a yellow oil.

Aufarbeitung

  1. stirringstirred for a further 16 h
  2. additionThe mixture was poured onto a flash column
  3. washeluted with ethyl acetate/hexane (40:60)

Quellen und Nachweise

ORD-Eintrag
ord-da9fb2defc484709833ce3eac5f1f837
Quelldatensatz
uspto-grants-2003_04
Patentnummer
US06541491B1

Notizen zur Reaktion

Wird geladen…