反应详情

A 2.0 M hexanes solution of trimethylsilyldiazomethane (11.8 mL, 23.62 mMol) was added dropwise to a stirring solution of 5-bromo-2-tert-butyl-pyrimidine-4-carboxylic acid (6.12 g, 23.62 mMol) in 9:1 benzene/methanol (100 mL), and the reaction was stirred for 2 days. TLC analysis showed that the reaction was complete, so the mixture was concentrated in-vacuo. The residue was dissolved in ethyl acetate (100 mL), washed with water (3×20 mL), dried over sodium sulfate, then concentrated in-vacuo. Purified over silica gel, eluting with 10% ethyl acetate/hexanes, to yield 5.2 g of a colorless oil as product. MS (ES+)=273,275 (M+H)+. Yield=81%.

1. concentrationwas concentrated in-vacuo
2. dissolutionThe residue was dissolved in ethyl acetate (100 mL)
3. washwashed with water (3×20 mL)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in-vacuo
6. customPurified over silica gel
7. washeluting with 10% ethyl acetate/hexanes