Ethanol → HCID 59515926, Verbindung

HRID 1161288Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1161288
[C:1]([O:4][CH2:5][CH2:6][NH:7][C:8]1[C:9]([N+:25]([O-])=O)=[C:10]2[C:15](=[CH:16][CH:17]=1)[C:14](=[O:18])[N:13]([CH2:19][CH2:20][O:21][C:22](=[O:24])[CH3:23])[CH:12]=[CH:11]2)(=[O:3])[CH3:2].C(O)C.[Cl-].[NH4+].O>[Fe].C(Cl)Cl>[C:1]([O:4][CH2:5][CH2:6][NH:7][C:8]1[C:9]([NH2:25])=[C:10]2[C:15](=[CH:16][CH:17]=1)[C:14](=[O:18])[N:13]([CH2:19][CH2:20][O:21][C:22](=[O:24])[CH3:23])[CH:12]=[CH:11]2)(=[O:3])[CH3:2]

Komponenten

7

Edukt 4

HCID 702EthanolHCID 962WaterHCID 25517Ammonium ChlorideHCID 595159322-(2-(2-Acetoxyethyl)-5-nitro-1-oxo-1,2-dihydroisoquinolin-6-ylamino)ethyl acetate

Produkt 1

HCID 59515926HCID 59515926, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A mixture of 2-(2-(2-acetoxyethyl)-5-nitro-1-oxo-1,2-dihydroisoquinolin-6-ylamino)ethyl acetate (350 mg, 0.00093 mol), ethanol (20 mL, 0.3 mol), ammonium chloride (496.1 mg, 0.009275 mol) and water (10 mL, 0.6 mol) was added at 85° C. Iron (207 mg, 0.00371 mol) was added in two portions five minutes apart and the reaction was stirred at that temperature for 1 hour. The reaction mixture was then poured into methylene chloride (100 mL) and the layers were separated and the organic layer was washed with brine and dried over sodium sulfate. The solvent was removed under reduced pressure and used for the next reaction without purification. MS m/z=348.5 (M+H).

Aufarbeitung

  1. additionwas added at 85° C
  2. customthe layers were separated
  3. washthe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. customThe solvent was removed under reduced pressure
  6. customused for the next reaction without purification

Quellen und Nachweise

ORD-Eintrag
ord-eb025335bb97488d810a1b8adc44b24e
Quelldatensatz
uspto-grants-2010_10
Patentnummer
US07816371B2

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