反应详情

温度

0 °C

A suspension of 5-(2-oxo-pyrrolidin-1-yl)-isophthalic acid monomethyl ester (A75) (200 mg, 0.76 mmol, 1 equiv) in THF (20 ml) was cooled to 0° C. and treated with BH3-Me2S (2M solution in THF, 0.64 ml, 1.28 mmol, 1.3 equiv). The resulting mixture was refluxed for 1 h and then cooled to room temperature. MeOH (5 ml) was added and the resulting mixture was concentrated in vacuo. The residue was diluted with AcOEt (50 ml) and the resulting solution was washed with saturated aqueous NaHCO3 solution (30 ml) and 2N aqueous HCl solution (30 ml), dried over MgSO4 and concentrated in vacuo to give 3-hydroxymethyl-5-(2-oxo-pyrrolidin-1-yl)-benzoic acid methyl ester (B76) (70 mg, 37%) as a pale yellow oil.

1. temperatureThe resulting mixture was refluxed for 1 h
2. temperaturecooled to room temperature
3. concentrationthe resulting mixture was concentrated in vacuo
4. additionThe residue was diluted with AcOEt (50 ml)
5. washthe resulting solution was washed with saturated aqueous NaHCO3 solution (30 ml) and 2N aqueous HCl solution (30 ml)
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo