Ethanol → 5-(6-Phenyl-7H-pyrrolo[2,3-d]pyrimidin-4-ylsulfanyl)-thiophen-2-ylamine
Reaktionsgleichung
[Cl-].[NH4+].CN(C)C=O.C(O)C.[N+:11]([C:14]1[S:18][C:17]([S:19][C:20]2[C:21]3[CH:28]=[C:27]([C:29]4[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=4)[NH:26][C:22]=3[N:23]=[CH:24][N:25]=2)=[CH:16][CH:15]=1)([O-])=O>[Fe].O1CCCC1.O>[C:29]1([C:27]2[NH:26][C:22]3[N:23]=[CH:24][N:25]=[C:20]([S:19][C:17]4[S:18][C:14]([NH2:11])=[CH:15][CH:16]=4)[C:21]=3[CH:28]=2)[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1Komponenten
8
Edukt 4
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 3
Reaktionsbedingungen
- Temperatur
- 90 °C
Versuchsvorschrift
After adding 543 mg of iron powder, 1.06 g of ammonium chloride, 10 ml of dimethylformamide, 20 ml of ethanol and 5 ml of water to the 4-(5-nitro-2-thiophenylsulfanyl)-6-phenyl-7H-pyrrolo[2,3-d]pyrimidine synthesized in Production Example 162-1, the mixture was stirred at 90° C. for 2 hours, 30 ml of tetrahydrofuran was added, and then the mixture was returned to room temperature and filtered with celite, and ethyl acetate and water were added to the filtrate for liquid separation and extraction. The organic layer was dried over anhydrous sodium sulfate, filtered with plug cotton and concentrated to dryness to obtain 435 mg of the title compound.
Aufarbeitung
- customsynthesized in Production Example 162-1
- customwas returned to room temperature
- filtrationfiltered with celite, and ethyl acetate and water
- additionwere added to the filtrate for liquid separation and extraction
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- filtrationfiltered with plug cotton
- concentrationconcentrated to dryness
Quellen und Nachweise
- ORD-Eintrag
- ord-58cc322241c74e3ca6b3357f838ec2eb
- Quelldatensatz
- uspto-grants-2013_02
- Patentnummer
- US08372981B2
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