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Acetic Anhydride → HCID 69497897, Verbindung

HRID 460643
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 460643
[Cl:1][C:2]1[CH:3]=[C:4]([CH:9]2[CH2:14][CH2:13][N:12]([CH2:15][C@H:16]([OH:34])[CH2:17][O:18][C:19]3[C:27]4[CH:26]=[C:25]([C:28]5[O:29][C:30]([CH3:33])=[N:31][N:32]=5)[O:24][C:23]=4[CH:22]=[CH:21][CH:20]=3)[CH2:11][CH2:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].[C:35](OC(=O)C)(=[O:37])[CH3:36]>N1C=CC=CC=1>[ClH:1].[C:35]([O:34][C@@H:16]([CH2:15][N:12]1[CH2:11][CH2:10][CH:9]([C:4]2[CH:5]=[CH:6][C:7]([Cl:8])=[C:2]([Cl:1])[CH:3]=2)[CH2:14][CH2:13]1)[CH2:17][O:18][C:19]1[C:27]2[CH:26]=[C:25]([C:28]3[O:29][C:30]([CH3:33])=[N:31][N:32]=3)[O:24][C:23]=2[CH:22]=[CH:21][CH:20]=1)(=[O:37])[CH3:36]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 7918Acetic AnhydrideHCID 9806065MIN-117

Produkt 1

HCID 69497897HCID 69497897, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

(S)-1-(4-(3,4-Dichlorophenyl)piperidino)-3-(2-(5-methyl-1,3,4-oxadiazol-2-yl)benzo(b)furan-4-yloxy)-2-propanol (1.0 g) was dissolved in pyridine (20 ml) and acetic anhydride (10 ml), and the mixture was left standing at room temperature for 12 hr. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (chloroform/methanol). The obtained oil was dissolved in ethanol and a solution of hydrogen chloride in ether was added. The precipitated crystals were collected by filtration and dried to give the title compound (0.58 g) as pale-yellow crystals, melting point 163–166° C. (decomposition)

Aufarbeitung

  1. customThe solvent was evaporated under reduced pressure
  2. customthe residue was purified by silica gel column chromatography (chloroform/methanol)
  3. dissolutionThe obtained oil was dissolved in ethanol
  4. additiona solution of hydrogen chloride in ether was added
  5. filtrationThe precipitated crystals were collected by filtration
  6. customdried

Quellen und Nachweise

ORD-Eintrag
ord-bc1aa9e658ef4ceb8ac4c23e21ab2830
Quelldatensatz
uspto-grants-2007_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07196199B2

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