HRID356539

反应详情

EQUATION

反应方程式

HRID 356539 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The title compound was prepared as described in General Method 9 from 6-cyclohexyl-4-hydroxy-6-[2-(4-hydroxy-phenyl)-ethyl]-5,6-dihydro-pyran-2-one (156 mg, 0.499 mmol; prepared in Example NN), toluene-4-thiosulfonic acid S-(2-tert-butyl-4-ethylsulfamoyloxy-5-methyl-phenyl) ester (prepared in Example VVV; 250 mg, 0.546 mmol), K2CO3 (303 mg, 2.195 mmol), and DMF (4 mL). The reaction was stirred at room temperature for 2.5 hours and then worked up in the usual manner. The crude product was flash chromatographed using CH2Cl2 :MeOH (98:2 to 97:3) to give the desired product as a amorphous solid. 1H NMR (CDCl3) δ 1.0-2.1 (m, 16 H), 1.55 (s, 9 H), 2.00 (s, 3 H), 2.6-2.7 (m, 3 H), 3.10 (d, 1 H), 3.3-3.4 (m, 2 H), 4.96 (t, 1 H), 6.70-6.78 (d, s, 3 H), 6.93 (d, 2 H), 7.29 (s, 1 H).

WORKUP

后处理

  1. customThe title compound was prepared
  2. customchromatographed