Lithium Hydroxide → HCID 68581174, Verbindung

HRID 2234009Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2234009
[Cl:1][C:2]1[C:6]([Cl:7])=[C:5]([CH3:8])[NH:4][C:3]=1[C:9]([NH:11][CH:12]1[CH2:17][CH2:16][N:15]([C:18]2[S:19][C:20]([C:35]([O:37]CC)=[O:36])=[C:21]([CH2:23][N:24]3[C:32](=[O:33])[C:31]4[C:26](=[CH:27][CH:28]=[CH:29][CH:30]=4)[C:25]3=[O:34])[N:22]=2)[CH2:14][CH2:13]1)=[O:10].[Li+].[OH-:41]>C1COCC1.O>[C:32]([C:31]1[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=1[C:25]([NH:24][CH2:23][C:21]1[N:22]=[C:18]([N:15]2[CH2:16][CH2:17][CH:12]([NH:11][C:9]([C:3]3[NH:4][C:5]([CH3:8])=[C:6]([Cl:7])[C:2]=3[Cl:1])=[O:10])[CH2:13][CH2:14]2)[S:19][C:20]=1[C:35]([OH:37])=[O:36])=[O:34])([OH:41])=[O:33]

Komponenten

5

Edukt 2

HCID 3939Lithium HydroxideHCID 68579992Ethyl 2-(4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)-4-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)methyl]-1,3-thiazole-5-carboxylate

Produkt 1

HCID 68581174HCID 68581174, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Ethyl 2-(4-{[(3,4-dichloro-5-methyl-1H-pyrrol-2-yl)carbonyl]amino}piperidin-1-yl)-4-[(1,3-dioxo-1,3-dihydro-2H-isoindol-2-yl)methyl]-1,3-thiazole-5-carboxylate (Example 277; 194 mg, 0.32 mmol) in anhydrous THF (2 ml) was added 2 N LiOH (0.82 ml). The mixture was stirred at room temperature for 4 h. The mixture was acidified to pH 3 and the precipitate that formed was diluted with water and extracted with EtOAc, dried over Na2SO4 and concentrated in vacuo to give the title compound (160 mg).

Aufarbeitung

  1. customthe precipitate that formed
  2. extractionextracted with EtOAc
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-789405b67adb4d9d8780be4c43f58913
Quelldatensatz
uspto-grants-2010_05
Patentnummer
US07709503B2

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