HRID2380572

反应详情

EQUATION

反应方程式

HRID 2380572 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 720 mg (2.0 mmol) of 3[[(4-methylphenyl)sulfonyl]oxy]cyclobutanemethanol, benzoate ester (95% trans isomer and 5% cis isomer) in 20 ml of dry dimethylformamide under nitrogen was added adenine (405 mg, 3 mmol), 18-crown-6 (528 mg, 2 mmol), and potassium carbonate (414 mg, 3 mmol). The mixture was stirred at 110° for 18 hours and then concentrated in vacuo to a residue. Water was added and the suspension was adjusted to pH 7.0 using 1N hydrochloric acid. Removal of solvent in vacuo gave a residue, which was chromatographed over 200 ml of LPS-1 silica gel using 4% methanol in dichloromethane to give 430 mg of desired product as a white solid.

WORKUP

后处理

  1. concentrationconcentrated in vacuo to a residue
  2. additionWater was added
  3. customRemoval of solvent in vacuo
  4. customgave a residue, which
  5. customwas chromatographed over 200 ml of LPS-1 silica gel using 4% methanol in dichloromethane