Dimethyl Sulfoxide → 1-[6-(4-Bromo-2-chloro-phenylamino)-7-fluoro-3H-benzoimidazol-5-yl]-2-methoxymethoxy-ethanone

To a solution of oxalyl chloride (0.11 mL, 0.22 mmol) in CH2Cl2 (1 mL) at −78° C. is added DMSO (0.016 mL, 0.22 mmol). After stirring for 3 minutes, a solution of 1-[6-(4-bromo-2-chloro-phenylamino)-7-fluoro-3H-benzoimidazol-5-yl]-2-methoxymethoxy-ethanol 10l (25 mg, 0.056 mmol) in methylene chloride (1 mL) is added. The resulting solution is stirred for 30 minutes at −78° C. TEA (0.1 mL, 0.71 mmol) is added. The reaction mixture is slowly warmed to room temperature, stirred for 5 minutes at room temperature, and diluted with water and CH2Cl2. The organic layer is separated, dried over MgSO4, filtered, and concentrated to give the crude product which is directly used without further purification.

1. stirringThe resulting solution is stirred for 30 minutes at −78° C
2. stirringstirred for 5 minutes at room temperature
3. customThe organic layer is separated
4. dry with materialdried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated

ORD 기록

ord-4775b9c5967843e29d6b2f19269203f9

출처 데이터셋

uspto-grants-2010_11

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07842816B2