Reaktionsgleichung
C(N(C(C)C)CC)(C)C.[CH:10]([CH2:12][C:13]([OH:15])=O)=[CH2:11].N1C2C=CC=C(O[P+](N(C)C)(N(C)C)N(C)C)C=2N=N1.F[P-](F)(F)(F)(F)F.Cl.Cl.[N:45]1[C:53]2[CH2:52][CH2:51][NH:50][CH2:49][C:48]=2[S:47][C:46]=1[NH:54][C:55]([NH2:57])=[NH:56].[OH-].[Na+]>CN(C)C=O>[C:13]([N:50]1[CH2:51][CH2:52][C:53]2[N:45]=[C:46]([NH:54][C:55]([NH2:57])=[NH:56])[S:47][C:48]=2[CH2:49]1)(=[O:15])[CH2:12][CH:10]=[CH2:11]Komponenten
7
Versuchsvorschrift
Diisopropylethylamine (0.22 mmol), vinyl acetic acid (0.11 mmol) and benzotriazolyloxy-tris-(dimethylamino)phosphonium-hexafluorophosphate (0.11 mmol) are added successively to a stirred suspension of N-(4,5,6,7-tetrahydro-thiazolo[5,4-c]pyridine-2-yl)-guanidine-dihydrochloride (0.1 mmol) in dimethylformamide (0.7 mL), and the reaction mixture is stirred for 16 hours at room temperature. After the addition of 2M caustic soda solution (1 ml) there is extraction with ethyl acetate. The combined organic phases produce the pure title compound after drying over sodium sulphate and concentrating to dryness.
Aufarbeitung
- extractionextraction with ethyl acetate
Quellen und Nachweise
- ORD-Eintrag
- ord-fecbe090558448a4a06f30a565bfc4fc
- Quelldatensatz
- uspto-grants-2010_06
- Patentnummer
- US07727979B2
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