Hydrochloric Acid → HCID 68676153, Verbindung

HRID 643150

Reaktionsgleichung

Reaktionsgleichung von HRID 643150
[Li+].[OH-].[NH2:3][C:4]1[C:36]([C:37]([F:40])([F:39])[F:38])=[CH:35][C:7]([CH2:8][C@@H:9]([CH2:14][C:15]([N:17]2[CH2:22][CH2:21][CH:20]([N:23]3[CH2:32][C:31]4[C:26](=[CH:27][CH:28]=[C:29]([OH:33])[CH:30]=4)[NH:25][C:24]3=[O:34])[CH2:19][CH2:18]2)=[O:16])[C:10]([O:12]C)=[O:11])=[CH:6][C:5]=1[Cl:41].Cl>O.C1COCC1>[NH2:3][C:4]1[C:36]([C:37]([F:39])([F:38])[F:40])=[CH:35][C:7]([CH2:8][C@@H:9]([CH2:14][C:15]([N:17]2[CH2:22][CH2:21][CH:20]([N:23]3[CH2:32][C:31]4[C:26](=[CH:27][CH:28]=[C:29]([OH:33])[CH:30]=4)[NH:25][C:24]3=[O:34])[CH2:19][CH2:18]2)=[O:16])[C:10]([OH:12])=[O:11])=[CH:6][C:5]=1[Cl:41]

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 69071695methyl (S)-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-4-[4-(6-hydroxy-2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidin-1-yl]-4-oxo-butanoate

Produkt 1

HCID 68676153HCID 68676153, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittel2×HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A solution of 144 mg (6.00 mmol) LiOH in 15 mL water was added to a solution of 2.30 g (4.04 mmol) methyl (S)-2-(4-amino-3-chloro-5-trifluoromethyl-benzyl)-4-[4-(6-hydroxy-2-oxo-1,4-dihydro-2H-quinazolin-3-yl)-piperidin-1-yl]-4-oxo-butanoate in 30 mL THF and the reaction mixture was stirred for 1 h at RT. The organic solvent was eliminated i.vac., the residue was diluted with 50 mL water and acidified with 1 M HCl. The precipitate formed was filtered, washed with 10 mL water and dried at 50° C.

Aufarbeitung

  1. customThe precipitate formed
  2. filtrationwas filtered
  3. washwashed with 10 mL water
  4. customdried at 50° C.

Quellen und Nachweise

ORD-Eintrag
ord-2bce32c587894f1eb77fea9c6714f8d1
Quelldatensatz
uspto-grants-2010_04
Patentnummer
US07696209B2

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