Methyl iodide → 5-(2-bromo-4-chloro-6-fluoro-phenyl)-1-methyl-1H-tetrazole

A mixture of 5-(2-bromo-4-chloro-6-fluoro-phenyl)-2H-tetrazole (4.15 g, 14.95 mmol), K2CO3 (3.1 g, 22.43 mmol) and iodomethane (1.3 ml, 20.94 mmol) in DMF (30 ml) was stirred at 25° C. for 3 h. The mixture was partitioned between EtOAc (80 ml) and water (60 ml), the organic layer was separated, washed with water and brine, dried with Na2SO4 and concentrated. The remaining residue was purified by chromatography (silica gel; hexane/EtOAc 100:0-90:10) to obtain 5-(2-bromo-4-chloro-6-fluoro-phenyl)-1-methyl-1H-tetrazole as pale yellow solid (1.5 g, 35%) and the title compound as reddish liquid (1.7 g, 39%). MS: 291.0 [M+H]+.

1. customThe mixture was partitioned between EtOAc (80 ml) and water (60 ml)
2. customthe organic layer was separated
3. washwashed with water and brine
4. dry with materialdried with Na2SO4
5. concentrationconcentrated
6. customThe remaining residue was purified by chromatography (silica gel; hexane/EtOAc 100:0-90:10)

ORD 기록

ord-7d3678795d8c4617949b03ee63bb20e7

출처 데이터셋

uspto-grants-2014_12

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08912221B2