6-amino-4-methyl-3,4-dihydro-2H-1,4-benzoxazin-3-one → HCID 59377423, Verbindung

Tetra-tert-butyl ammonium bromide (6.77 g, 14.04 mmol) was added to a solution of 6-amino-4-methyl-4H-benzo[1,4]oxazin-3-one (2.5 g, 14.04 mmol) in methylene chloride (100 ml) and MeOH (50 ml). The mixture was stirred at room temperature for 20 minutes, then quenched with aqueous sodium bisulfite solution. The mixture was extracted with methylene chloride, and the combined organic extracts were dried over MgSO4, filtered, concentrated under reduced pressure and purified via column chromatography to give 1.30 g of 6-amino-7-bromo-4-methyl-4H-benzo[1,4]oxazin-3-one as a light yellow solid, 40%.

1. customquenched with aqueous sodium bisulfite solution
2. extractionThe mixture was extracted with methylene chloride
3. dry with materialthe combined organic extracts were dried over MgSO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. custompurified via column chromatography

ORD-Eintrag

ord-542b3f87ce0840ea9a032193ac67d623

Quelldatensatz

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08372865B2