Calcium Chloride → N-(5-amino-4'-methoxybiphenyl-3-yl)acetamide

HRID 64134Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 64134
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:14]=[C:13]([N+:15]([O-])=O)[CH:12]=[C:11]([NH:18][C:19](=[O:21])[CH3:20])[CH:10]=2)=[CH:5][CH:4]=1.[Cl-].[Ca+2].[Cl-]>C(O)C.[Fe]>[NH2:15][C:13]1[CH:12]=[C:11]([NH:18][C:19](=[O:21])[CH3:20])[CH:10]=[C:9]([C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=2)[CH:14]=1

Komponenten

5

Edukt 2

HCID 5284359Calcium ChlorideHCID 89500151N-(4'-methoxy-5-nitrobiphenyl-3-yl)acetamide

Produkt 1

HCID 89500101N-(5-amino-4'-methoxybiphenyl-3-yl)acetamideAusbeute 87 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 23925IronKatalysatorHCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
100 °C

Versuchsvorschrift

To a solution of N-(4′-methoxy-5-nitrobiphenyl-3-yl)acetamide (4 g, 13.98 mmol) in ethanol (50 ml) were added calcium chloride (3.1 g, 27.96 mmol, 2 eq.) and iron powder (1.45 g, 27.96 mmol, 2 eq.) and the mixture was heated at 100° C. for 2 h and filtered. The filtrate was diluted with water and extracted as in Example 1(d). The solvent was distilled off to afford the product in 87% yield (3.1 g).

Aufarbeitung

  1. filtrationfiltered
  2. additionThe filtrate was diluted with water
  3. extractionextracted as in Example 1(d)
  4. distillationThe solvent was distilled off
  5. customto afford the product in 87% yield (3.1 g)

Quellen und Nachweise

ORD-Eintrag
ord-2466cabf962a464c8397abc5d9bda431
Quelldatensatz
uspto-grants-2016_09
Patentnummer
US09447091B2

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