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Lithium Hydroxide → HCID 68793468, Verbindung

HRID 1161008
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1161008
[OH-].[Li+].[CH3:3][CH:4]([CH3:46])[CH2:5][CH2:6][N:7]([CH2:41][CH2:42][CH:43]([CH3:45])[CH3:44])[C:8]([C:10]1[CH:11]=[CH:12][C:13]2[N:17]=[C:16]([NH:18][C:19]3[CH:28]=[CH:27][C:22]([C:23]([O:25]C)=[O:24])=[CH:21][CH:20]=3)[N:15]([CH2:29][CH2:30][CH2:31][NH:32][C:33]([O:35][C:36]([CH3:39])([CH3:38])[CH3:37])=[O:34])[C:14]=2[CH:40]=1)=[O:9]>O1CCCC1.O.C(OCC)C>[CH3:44][CH:43]([CH3:45])[CH2:42][CH2:41][N:7]([CH2:6][CH2:5][CH:4]([CH3:46])[CH3:3])[C:8]([C:10]1[CH:11]=[CH:12][C:13]2[N:17]=[C:16]([NH:18][C:19]3[CH:28]=[CH:27][C:22]([C:23]([OH:25])=[O:24])=[CH:21][CH:20]=3)[N:15]([CH2:29][CH2:30][CH2:31][NH:32][C:33]([O:35][C:36]([CH3:39])([CH3:37])[CH3:38])=[O:34])[C:14]=2[CH:40]=1)=[O:9]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 2

HCID 3939Lithium HydroxideHCID 68792031methyl 4-[(6-{[bis(3-methylbutyl)amino]carbonyl}-1-{3-[(tert-butoxycarbonyl) amino]propyl}-1H-benzimidazol-2-yl)amino]benzoate

Produkt 1

HCID 68793468HCID 68793468, VerbindungAusbeute 79 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 3283
Diethyl Ether
Lösungsmittel
HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Lithium hydroxide (141 mg, 5 eq) is added to methyl 4-[(6-{[bis(3-methylbutyl)amino]carbonyl}-1-{3-[(tert-butoxycarbonyl)amino]propyl}-1H-benzimidazol-2-yl)amino]benzoate prepared according to reaction diagram A, Example A1, (405 mg, 1 eq) in a mixture of tetrahydrofuran (4 ml) and water (3 ml). The mixture is heated under reflux for 18 hours then cooled down to ambient temperature and concentrated under reduced pressure at 40° C. Dichloromethane (50 ml) and water (20 ml) are added to the residue. The mixture is acidified by the addition of acetic acid to pH 5. After decantation and extractions, the combined organic phases are dried over sodium sulphate and concentrated under reduced pressure. The solid obtained is taken up in ethyl ether in order to produce the expected compound (309 mg; 79%).

Aufarbeitung

  1. customprepared
  2. customaccording to reaction diagram A, Example A1, (405 mg, 1 eq)
  3. temperatureThe mixture is heated
  4. temperatureunder reflux for 18 hours
  5. concentrationconcentrated under reduced pressure at 40° C
  6. additionDichloromethane (50 ml) and water (20 ml) are added to the residue
  7. additionThe mixture is acidified by the addition of acetic acid to pH 5
  8. extractionAfter decantation and extractions
  9. dry with materialthe combined organic phases are dried over sodium sulphate
  10. concentrationconcentrated under reduced pressure
  11. customThe solid obtained

Quellen und Nachweise

ORD-Eintrag
ord-24484085238b4e5cb9448616bdc53122
Quelldatensatz
uspto-grants-2010_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07816539B2

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