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Dimethylformamide → HCID 86677428, Verbindung

HRID 2089709
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2089709
C(O)(=O)C.[C:5]([C:8]1[CH:13]=[CH:12][C:11]([NH:14][C@@H:15]([C:32]2[N:36]=[C:35]([O:37][CH2:38][O:39][C:40]([O:42][CH:43]([CH3:45])[CH3:44])=[O:41])[N:34]([C:46]3[N:51]=[CH:50][CH:49]=[CH:48][N:47]=3)[N:33]=2)[C:16]2[C:17]([F:31])=[C:18]([CH:26]=[C:27]([O:29][CH3:30])[CH:28]=2)[O:19][CH2:20][CH2:21][O:22][C:23](=[O:25])[CH3:24])=[CH:10][CH:9]=1)(=[NH:7])[NH2:6].CN(C=O)C.[N+](C1C=CC([O:66][C:67](=O)[O:68][CH2:69][CH:70]([CH3:72])[CH3:71])=CC=1)([O-])=O.C(N(CC)CC)C>O.C(OCC)(=O)C>[NH2:7][C:5](=[N:6][C:67]([O:68][CH2:69][CH:70]([CH3:72])[CH3:71])=[O:66])[C:8]1[CH:9]=[CH:10][C:11]([NH:14][C@@H:15]([C:32]2[N:36]=[C:35]([O:37][CH2:38][O:39][C:40]([O:42][CH:43]([CH3:45])[CH3:44])=[O:41])[N:34]([C:46]3[N:47]=[CH:48][CH:49]=[CH:50][N:51]=3)[N:33]=2)[C:16]2[C:17]([F:31])=[C:18]([CH:26]=[C:27]([O:29][CH3:30])[CH:28]=2)[O:19][CH2:20][CH2:21][O:22][C:23](=[O:25])[CH3:24])=[CH:12][CH:13]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 4

HCID 6228DimethylformamideHCID 8471TriethylamineHCID 64292502-Methylpropyl (4-nitrophenyl) carbonateHCID 86677426Acetic acid 2-{3-[(R)-(4-carbamimidoylphenylamino)-(5-isopropoxycarbonyloxymethoxy-1-pyrimidin-2-yl-1H-[1,2,4]triazol-3-yl)methyl]-2-fluoro-5-methoxyphenoxy}ethyl ester acetic acid salt

Produkt 1

HCID 86677428
HCID 86677428, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a mixture of Acetic acid 2-{3-[(R)-(4-carbamimidoylphenylamino)-(5-isopropoxycarbonyloxymethoxy-1-pyrimidin-2-yl-1H-[1,2,4]triazol-3-yl)methyl]-2-fluoro-5-methoxyphenoxy}ethyl ester acetic acid salt (23 mg) obtained in Example 67a and DMF (1 ml), carbonic acid isobutyl ester 4-nitrophenyl ester [CAS No. 112240-73-0] (10 mg) and triethylamine (50 μL) were added, and the resulting mixture was stirred at room temperature for 64 h. Ethyl acetate and water were added to the mixture, and the organic layer was collected. The organic layer was sequentially washed with water and with saturated aqueous sodium chloride solution, and dried over anhydrous magnesium sulfate. The desiccant was filtered off, and the filtrate obtained was concentrated under reduced pressure. The residue obtained was purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate) to obtain the captioned compound (14.99 mg).

Aufarbeitung

  1. customthe organic layer was collected
  2. washThe organic layer was sequentially washed with water and with saturated aqueous sodium chloride solution
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationThe desiccant was filtered off
  5. customthe filtrate obtained
  6. concentrationwas concentrated under reduced pressure
  7. customThe residue obtained
  8. customwas purified by silica gel column chromatography (mixed solvent of heptane-ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-55f4df05226f4706b926d793f4dcf12d
Quelldatensatz
uspto-grants-2013_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08436009B2

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