Sodium Hydroxide → 6-Bromoisoquinolin-3-Amine
Reaktionsgleichung
[Br:1][C:2]1[CH:18]=[CH:17][C:5]([CH2:6][NH:7][C:8](=[NH:16])[CH:9](OCC)OCC)=[CH:4][CH:3]=1.[OH-].[Na+]>S(=O)(=O)(O)O>[Br:1][C:2]1[CH:18]=[C:17]2[C:5](=[CH:4][CH:3]=1)[CH:6]=[N:7][C:8]([NH2:16])=[CH:9]2Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
N-(4-bromobenzyl)-2,2-diethoxyacetimidamide (1.53 g, 4.85 mmol) in sulfuric acid (4 mL, 95-98%) was heated at 40 C for 14 h. The mixture was neutralized with 1M NaOH to pH 7 and the resulting suspension was filtered. The residue was purified by silica gel chromatography with 20-55% ethyl acetate in hexanes. The desired fractions were concentrated to give a brownish yellow solid (0.434 g, 40%). LCMS:R.T.=1.62; [M+2]+=225.1.
Aufarbeitung
- filtrationthe resulting suspension was filtered
- customThe residue was purified by silica gel chromatography with 20-55% ethyl acetate in hexanes
- concentrationThe desired fractions were concentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-1a3da4c8529e4a538ea99a6647f37791
- Quelldatensatz
- uspto-grants-2011_01
- Patentnummer
- US07863291B2
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