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With pyridine; methanesulfonyl chloride; In tetrahydrofuran; at 0 - 20℃; for 0.416667h;
To a solution of 3-methyl-2-oxo-butanoic acid sodium salt (1.03 g, 7.47 mmol) in THF (9.8 ml)were added alpha,alpha-dimethoxy benzenemethanol (2.05 g, 15.0 mmol) and pyridine (1.55 ml, 18.7 mmol).The mixture was cooled to 0 C, and methanesulfonyl chloride (700 muL, 8.97 mmol) was added. The reaction mixture was stirred for 25 min at room temperature before quenching with distilled water at 0 C. The resulting mixture was extracted with diethylether twice. The combined organic layers were washed with brine, dried over MgSO4, and concentrated in vacuo. Further purification was carriedout by silica gel column chromatography to give 13f (699.7 mg, 40%) as a colorless oil.
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