HRID481902

反应详情

EQUATION

反应方程式

HRID 481902 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-6,6-diphenyl-2H-pyran-2-one (0.250 g, 0.940 mmol), Et3N (0.13 mL, 0.94 mmol), benzoyl chloride (0.109 mL, 0.94 mmol), CH2Cl2 (2.0 mL), acetonitrile (5.0 mL), acetone cyanohydrin (0.01 mL, 0.09 mmol), Et3N (0.27 mL, 1.9 mmol), glacial acetic acid (10.0 mL), sodium cyanoborohydride (0.133 g, 2.11 mmol). Purification was achieved by submitting the final residue to column chromatograpy (SiO2, 4/1 hexane/ethyl acetate to 3/2 hexane/ethyl acetate) to provide a solid (0.105 g, 63°-65° C.). 1H NMR (400 MHz, DMSO-d6) δ11.136 (s, 1H), 7.501-7.280 (m, 11H), 6.997-6.932 (m, 2H), 6.566 (d, 2H, J=7 Hz), 3.530 (s, 2H), 3.432 (s, 2H),

WORKUP

后处理

  1. customPurification
  2. customto provide a solid (0.105 g, 63°-65° C.)