反应详情

To a solution of 5-bromo-3-thiophenecarboxylic acid (1 g, 4.85 mmol)[prepared according to J. Org. Chem. 1976, 41, 2350.], 1,1-dimethylethyl (2-amino-2-phenylethyl)carbamate (1.1 g, 4.85 mmol)[from Preparation 1] and diisopropylethyl amine (2.5 mL, 14.60 mmol) in DCM (50 mL) at 25° C. was added PyBrOP (2.5 g, 5.30 mmol) in one portion. After 16 h, the solution was partitioned between H2O and washed with DCM. The combined organic fractions were dried (Na2SO4), concentrated and purified via column chromatography (silica, 1% MeOH in DCM) affording the title compound (1.4 g, 68%) as a white solid: LC-MS (ES) m/z=426 (M+H)+.

1. customthe solution was partitioned between H2O
2. washwashed with DCM
3. dry with materialThe combined organic fractions were dried (Na2SO4)
4. concentrationconcentrated
5. custompurified via column chromatography (silica, 1% MeOH in DCM)