HRID481908

反应详情

EQUATION

反应方程式

HRID 481908 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The title compound was prepared as described in General Method 8 using the following: 5,6-dihydro-4-hydroxy-6-phenyl-6-(2-phenylethyl)-2H-pyran-2-one (0.300 g, 1.02 mmol), Et3N (0.15 mL, 1.1 mmol), 2-trifluoromethylbenzoyl chloride (0.21 mL, 1.02 mmol), CH2Cl2 (4.0 mL), acetonitrile (4.0 mL), acetone cyanohydrin (0.04 mL, 0.47 mmol), Et3N (0.29 mL, 2.1 mmol), glacial acetic acid (3.0 mL), sodium cyanoborohydride (0.20 g, 3.1 mmol). Purification was achieved by submitting the final residue to column chromatograpy (SiO2, 100% CH2Cl2 to 1% MeOH in CH2Cl2) to provide an oil (0.102 g). 1H NMR (400 MHz, DMSO-d6) δ11.21 (bs, 1H), 7.584 (d, 1H, J=8 Hz), 7.457-7.030 (m, 12H), 6.179 (d, 1H, J=7.5 Hz), 3.594 (s, 2H), 3.362 (d, 1H, J=17 Hz), 3.249 (d, 1H, J=17 Hz), 2.686-2.603 (m, 1H), 2.374-2.182 (m, 3H).

WORKUP

后处理

  1. customPurification