Methanol → 4'-[2-({8-[2-(Acetylamino)ethyl]-2-naphthyl}oxy)ethoxy]-[1,1'-biphenyl]-4-carboxylic acid

HRID 1373481Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1373481
[C:1]([NH:4][CH2:5][CH2:6][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:16]=1[CH:15]=[C:14]([O:17][CH2:18][CH2:19][O:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]3[CH:32]=[CH:31][C:30]([C:33]([O:35]C)=[O:34])=[CH:29][CH:28]=3)=[CH:23][CH:22]=1)[CH:13]=[CH:12]2)(=[O:3])[CH3:2].CO.O.[OH-].[Na+]>C1COCC1>[C:1]([NH:4][CH2:5][CH2:6][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:16]=1[CH:15]=[C:14]([O:17][CH2:18][CH2:19][O:20][C:21]1[CH:26]=[CH:25][C:24]([C:27]3[CH:32]=[CH:31][C:30]([C:33]([OH:35])=[O:34])=[CH:29][CH:28]=3)=[CH:23][CH:22]=1)[CH:13]=[CH:12]2)(=[O:3])[CH3:2]

Komponenten

6

Edukt 4

HCID 887MethanolHCID 962WaterHCID 14798Sodium HydroxideHCID 15540840Methyl 4'-[2-({8-[2-(acetylamino)ethyl]-2-naphthyl}oxy)ethoxy]-[1,1'-biphenyl]-4-carboxylate

Produkt 1

HCID 155408414'-[2-({8-[2-(Acetylamino)ethyl]-2-naphthyl}oxy)ethoxy]-[1,1'-biphenyl]-4-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

In a 100 ml round-bottomed flask, 19 mmol of the compound obtained in Example 1 are suspended in 25 ml of THF, and then 15 ml of methanol, 15 ml of water and 38 mmol of sodium hydroxide are added. The reaction mixture is maintained at ambient temperature with stirring for 10 hours. The solution is subsequently concentrated, poured into water and then acidified with 12M HCl. The precipitate obtained is filtered off, washed with water and recrystallised to yield the title product.

Aufarbeitung

  1. concentrationThe solution is subsequently concentrated
  2. additionpoured into water
  3. customThe precipitate obtained
  4. filtrationis filtered off
  5. washwashed with water
  6. customrecrystallised

Quellen und Nachweise

ORD-Eintrag
ord-b2091e56b218413f97fcb4194ca9bd8b
Quelldatensatz
uspto-grants-2007_01
Patentnummer
US07161035B2

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