Lithium hydroxide, monohydrate → 17-[2-(3-Isopropylpyrazol-1-yl)-7-methoxy-8-methylquinazolin-4-yloxy]-13-methyl-2,14-dioxo-3,13-diazatricyclo[13.3.0.04,6]octadec-7-ene-4-carboxylic acid

HRID 1443496Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1443496
O.[OH-].[Li+].C([O:6][C:7]([C:9]12[CH2:26][CH:25]1[CH:24]=[CH:23][CH2:22][CH2:21][CH2:20][CH2:19][N:18]([CH3:27])[C:17](=[O:28])[CH:16]1[CH:12]([CH2:13][CH:14]([O:29][C:30]3[C:39]4[C:34](=[C:35]([CH3:42])[C:36]([O:40][CH3:41])=[CH:37][CH:38]=4)[N:33]=[C:32]([N:43]4[CH:47]=[CH:46][C:45]([CH:48]([CH3:50])[CH3:49])=[N:44]4)[N:31]=3)[CH2:15]1)[C:11](=[O:51])[NH:10]2)=[O:8])C>O.C1COCC1>[CH:48]([C:45]1[CH:46]=[CH:47][N:43]([C:32]2[N:31]=[C:30]([O:29][CH:14]3[CH2:13][CH:12]4[CH:16]([C:17](=[O:28])[N:18]([CH3:27])[CH2:19][CH2:20][CH2:21][CH2:22][CH:23]=[CH:24][CH:25]5[C:9]([C:7]([OH:8])=[O:6])([NH:10][C:11]4=[O:51])[CH2:26]5)[CH2:15]3)[C:39]3[C:34](=[C:35]([CH3:42])[C:36]([O:40][CH3:41])=[CH:37][CH:38]=3)[N:33]=2)[N:44]=1)([CH3:50])[CH3:49]

Komponenten

5

Edukt 2

HCID 168937Lithium hydroxide, monohydrateHCID 68688284HCID 68688284, Verbindung

Produkt 1

HCID 6868954017-[2-(3-Isopropylpyrazol-1-yl)-7-methoxy-8-methylquinazolin-4-yloxy]-13-methyl-2,14-dioxo-3,13-diazatricyclo[13.3.0.04,6]octadec-7-ene-4-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of lithium hydroxide hydrate (796 mg, 18.6 mmol) in water (10 mL) was added to a stirred solution of the ester (145) (346 mg, 0.526 mmol) in THF (30 mL). After 5 days at room temperature, the reaction mixture was concentrated under vacuum. The pH was adjusted to 4 with 1N HCl and the resulting solution was successively extracted with AcOEt, washed with brine, dried (Na2SO4) and evaporated.

Aufarbeitung

  1. concentrationthe reaction mixture was concentrated under vacuum
  2. extractionthe resulting solution was successively extracted with AcOEt
  3. washwashed with brine
  4. dry with materialdried (Na2SO4)
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-456e7c9b35144961b7548638a99cd33f
Quelldatensatz
uspto-grants-2010_02
Patentnummer
US07659245B2

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