Ethyl Acetate → 1,1-Dimethylethyl N-[4-(bromomethyl)-2-pyridinyl]carbamate

Triphenylphosphine (970 mg, 3.7 mmol) and carbon tetrabromide (1.5 g, 4.6 mmol) were added to a solution of (2-tert-butoxycarbonylaminopyridin-4-yl)methanol (Reference compound No. 4-1, 690 mg, 3.1 mmol) in methylene chloride (20 mL) under ice-cooling, and the mixture was stirred for 2 hours at room temperature. Ethyl acetate (30 mL) was added to the reaction mixture, the whole was washed with saturated aqueous sodium hydrogen carbonate solution (20 mL) and brine (20 mL), and then dried over anhydrous magnesium sulfate. The organic layer was evaporated under reduced pressure, and the resulting solid was filtered off with ethyl acetate to give 550 mg of the title reference compound as a colorless solid. (Yield 62%)

1. washthe whole was washed with saturated aqueous sodium hydrogen carbonate solution (20 mL) and brine (20 mL)
2. dry with materialdried over anhydrous magnesium sulfate
3. customThe organic layer was evaporated under reduced pressure
4. filtrationthe resulting solid was filtered off with ethyl acetate
5. customto give 550 mg of the title reference compound as a colorless solid

ORDレコード

ord-0f5a3073906945fdb8b62484d3049fa9

出典データセット

uspto-grants-2009_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07544703B2