Reaktionsgleichung
[CH3:1][S:2][C:3]1[N:8]=[C:7]([NH:9][C:10]2([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[CH2:12][CH2:11]2)[C:6]([C:19]([O:21]CC)=[O:20])=[CH:5][N:4]=1>C1COCC1.O>[CH3:1][S:2][C:3]1[N:8]=[C:7]([NH:9][C:10]2([C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][CH:18]=3)[CH2:11][CH2:12]2)[C:6]([C:19]([OH:21])=[O:20])=[CH:5][N:4]=1Komponenten
4
Versuchsvorschrift
To a solution of ethyl 2-(methylthio)-4-(1-phenylcyclopropylamino)pyrimidine-5-carboxylate (crude from step 2) in THF (4 mL) was added LiOHH2O (150 mg, 3.57 mmol) in H2O (2 mL). The mixture was stirred at room temperature overnight. THF was removed under vacuum and the residue was acidified with 1N HCl, white solids precipitated out, which were collected by filtration, dried on vacuum to give 2-(methylthio)-4-(1-phenylcyclopropylamino)pyrimidine-5-carboxylic acid (646 mg). MS 302.3 (M+H).
Aufarbeitung
- customTHF was removed under vacuum
- customprecipitated out
- filtrationwhich were collected by filtration
- customdried on vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-be23b1820d3f489a97e26d40e4f451d1
- Quelldatensatz
- uspto-grants-2014_10
- Patentnummer
- US08853230B2
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