(4-Methoxy-benzyl)-[4-methyl-5-(2-morpholin-4-yl-pyrimidin-4-yl)-thiazol-2-yl]-amine → 4-Methyl-5-(2-morpholin-4-yl-pyrimidin-4-yl)-thiazol-2-ylamine
Reaktionsgleichung
COC1C=CC(C[NH:8][C:9]2[S:10][C:11]([C:15]3[CH:20]=[CH:19][N:18]=[C:17]([N:21]4[CH2:26][CH2:25][O:24][CH2:23][CH2:22]4)[N:16]=3)=[C:12]([CH3:14])[N:13]=2)=CC=1>FC(F)(F)C(O)=O.O>[CH3:14][C:12]1[N:13]=[C:9]([NH2:8])[S:10][C:11]=1[C:15]1[CH:20]=[CH:19][N:18]=[C:17]([N:21]2[CH2:26][CH2:25][O:24][CH2:23][CH2:22]2)[N:16]=1Komponenten
3
Edukt 1
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 75 °C
Versuchsvorschrift
A solution comprising (4-methoxy-benzyl)-[4-methyl-5-(2-morpholin-4-yl-pyrimidin-4-yl)-thiazol-2-yl]-amine (25c) (0.45 g, 1.13 mmol) in trifluoroacetic acid:water (95:5) (10 ml) is heated at 75° C. for days. The solvent is removed in vacuo and the crude residue is dissolved in ethyl acetate. The pH is adjusted to pH12 using 2N sodium hydroxide and the layers are separated. The aqueous layer is extracted with ethyl acetate (2×30 ml). The organic portions are combined and washed with brine (50 ml), dried over MgSO4 and concentrated in vacuo to yield the titled compound as a brown solid.
Aufarbeitung
- customThe solvent is removed in vacuo
- dissolutionthe crude residue is dissolved in ethyl acetate
- customthe layers are separated
- extractionThe aqueous layer is extracted with ethyl acetate (2×30 ml)
- washwashed with brine (50 ml)
- dry with materialdried over MgSO4
- concentrationconcentrated in vacuo
Quellen und Nachweise
- ORD-Eintrag
- ord-8c7f8a191e05474a866482fb25528157
- Quelldatensatz
- uspto-grants-2013_03
- Patentnummer
- US08404684B2
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