反应详情

The ester is formed according to the method of Molander et al. (J. Org. Chem. 68, 5534, (2003)). To a stirring suspension of potassium methyltrifluoroborate (629.0 mg, 5.2 mmol) Cs2CO3 (5.0 g, 15.5 mmol), PdCl2(dppf).CH2Cl2 (46.0 mg, 0.057 mmol), and triflate (46.3) (2.0 g, 5.7 mmol) in 50 mL THF is added water (5 mL) under an argon atmosphere. Stirring the mixture at reflux until TLC confirms the consumption of the starting material. The mixture is cooled to room temperature, and is diluted with water and extracted with ether. The combined organic layers are dried (MgSO4) and concentrated under reduced pressure. The residue is purified by column chromatography (silica, EtOAc/Hexane), to afford ester 46.4.

1. temperatureat reflux until TLC
2. customthe consumption of the starting material
3. additionis diluted with water
4. extractionextracted with ether
5. dry with materialThe combined organic layers are dried (MgSO4)
6. concentrationconcentrated under reduced pressure
7. customThe residue is purified by column chromatography (silica, EtOAc/Hexane)