Methanamine, N-methoxy-, hydrochloride (1:1) → HCID 64322489, Verbindung

Into a 1-L round-bottom flask, was placed a solution of 4-amino-3-bromobenzoic acid (50 g, 231.45 mmol, 1.00 equip) in N,N-dimethylformamide (500 mL), TEA (128 mL, 4.00 equip), HATU (106 g, 278.78 mmol, 1.20 equip), and methoxy(methyl)amine hydrochloride (45 g, 461.33 mmol, 2.00 equip). The resulting solution was stirred overnight at room temperature. The resulting solution was diluted with water (1 L). The resulting solution was extracted with ethyl acetate (1 L) and the organic layers combined and dried over anhydrous sodium sulfate. The solids were filtered out. The resulting mixture was concentrated under vacuum. The residue was applied onto a silica gel column with ethyl acetate/petroleum ether (1:2) to yield 4-amino-3-bromo-N-methoxy-N-methylbenzamide as a yellow solid. LCMS (ES, m/z) 259 [M+H]+

1. customInto a 1-L round-bottom flask, was placed
2. extractionThe resulting solution was extracted with ethyl acetate (1 L)
3. dry with materialdried over anhydrous sodium sulfate
4. filtrationThe solids were filtered out
5. concentrationThe resulting mixture was concentrated under vacuum

ORD-Eintrag

ord-8f26cd481f2e41fca6d00b7600702080

Quelldatensatz

uspto-grants-2016_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09266835B2