反应详情

To a solution of 1-bromo-3-chloro-5-nitrobenzene 52.A (10.23 g, 43 mmol, available from Synchem Inc), Pd2(dba)3 (0.79 g, 0.87 mmol) and CTC-QPhos (1.20 g, 1.40 mmol) in THF (100 mL) was added 2-tert-Butoxy-2-oxoethylzinc chloride (95 mL, 0.5M solution in diethyl ether, 48 mmol, available from Rieke Metals). The mixture was stirred for 3 hours at room temperature. The reaction was then quenched by adding water (100 mL), washed with 1N HCl solution (2×100 mL), concentrated and purified by using flash chromatography on silica gel (0-10% AcOEt/Hexanes) to afford tert-butyl 2-(3-chloro-5-nitrophenyl)acetate 52.B (9.60 g, 82% yield) as a light pink oil.

1. customThe reaction was then quenched
2. additionby adding water (100 mL)
3. washwashed with 1N HCl solution (2×100 mL)
4. concentrationconcentrated
5. custompurified