Sodium Bicarbonate → HCID 10362721, Verbindung

HRID 1271856Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1271856
C(OC(=O)[NH:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[NH:14][C:15]([C:17]1[S:21][C:20]2[CH:22]=[CH:23][C:24]([O:26][CH2:27][CH2:28][O:29][CH2:30][CH2:31][O:32][CH3:33])=[CH:25][C:19]=2[CH:18]=1)=[O:16])(C)(C)C.C(=O)(O)[O-].[Na+]>FC(F)(F)C(O)=O>[NH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[NH:14][C:15]([C:17]1[S:21][C:20]2[CH:22]=[CH:23][C:24]([O:26][CH2:27][CH2:28][O:29][CH2:30][CH2:31][O:32][CH3:33])=[CH:25][C:19]=2[CH:18]=1)=[O:16]

Komponenten

4

Edukt 2

HCID 516892Sodium BicarbonateHCID 86593875HCID 86593875, Verbindung

Produkt 1

HCID 10362721HCID 10362721, VerbindungAusbeute 62,8 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6422Trifluoroacetic acidLösungsmittel

Versuchsvorschrift

A solution of 80 mg (0.164 mmol) of [2-({5-[2-(2-Methoxy-ethoxy)-ethoxy]-benzo[b]thiophene-2-carbonyl}-amino)-phenyl]-carbamic acid tert-butyl ester (28) in 1.0 ml trifluoroacetic acid was stirred for 45 min at room temperature and then added to an aqueous solution of sodium bicarbonate. After extraction with ethyl acetate and removal of the solvent the residue was recrystallized from ethyl acetate/heptane to yield 40 mg (0.103 mmol) of the desired product (27) as white crystals, mp. 167–168° C.

Aufarbeitung

  1. extractionAfter extraction
  2. customwith ethyl acetate and removal of the solvent the residue
  3. customwas recrystallized from ethyl acetate/heptane

Quellen und Nachweise

ORD-Eintrag
ord-dca74ae1eaf148c1ae454ec44ad3f05b
Quelldatensatz
uspto-grants-2007_04
Patentnummer
US07208491B2

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