Ethanol → Ethyl 4-benzylamino-2-ethoxy-5-nitro-benzoate

HRID 578056Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 578056
[CH2:1]([NH:8][C:9]1[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:11](F)[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH2:24]([OH:26])[CH3:25].OS([O-])(=O)=O.[K+]>O>[CH2:1]([NH:8][C:9]1[C:19]([N+:20]([O-:22])=[O:21])=[CH:18][C:12]([C:13]([O:15][CH2:16][CH3:17])=[O:14])=[C:11]([O:26][CH2:24][CH3:25])[CH:10]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

Komponenten

5

Edukt 3

HCID 702Ethanol2×HCID 516920Potassium bisulfateHCID 67230873Ethyl 4-benzylamino-2-fluoro-5-nitro-benzoate

Produkt 1

HCID 67233615Ethyl 4-benzylamino-2-ethoxy-5-nitro-benzoate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

The product obtained at (655b) (15.5 g, 2.97 mmol) was combined with a mixture of potassium tert.-butylate (6.00 g, 53.5 mmol) and 400 mL ethanol, that was stirred at ambient temperature already for 15 min. After stirring for 1 h, 400 mL ethanol were added. After further 1 h of stirring, potassium tert.-butylate (500 mg, 4.46 mmol) was added. After further 1.5 h, the mixture was poured into water and acidified with KHSO4 (aq). After stirring for 20 min, the precipitate was filtered off, washed with water and dried at 55° C.

Aufarbeitung

  1. stirringAfter stirring for 1 h
  2. stirringAfter further 1 h of stirring
  3. waitAfter further 1.5 h
  4. stirringAfter stirring for 20 min
  5. filtrationthe precipitate was filtered off
  6. washwashed with water
  7. customdried at 55° C.

Quellen und Nachweise

ORD-Eintrag
ord-df6e1412688b4290a9c3ca04481397d0
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09040565B2

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