HRID2165444

反应详情

EQUATION

反应方程式

HRID 2165444 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

7 ml of a 1.65 M hexane solution of n-butyllithium was dissolved in 30 ml of anhydrous tetrahydrofuran. To the solution was added at -78° C a solution of 3.3 g of 1,4,5-trimethoxy-3-bromo-naphthalene (VI, R=OCH3) in 30 ml of anhydrous tetrahydrofuran. 2,5 g of 2-methoxy-carbonyl-5-(2-methyl-dioxolan-2-yl)-6-oxa -bicyclo[3,2,1]-octan-7-one, prepared as described in Example 3, was dissolved in 50 ml of anhydrous tetrahydrofuran and added to the reaction mixture. The reaction mixture was stood for 1 hour at -78° C and then quenched with acetic acid. The solvent was removed in vacuo. The residue was purified by silica gel column chromatograhy, giving 3 g (73% yield) of the title compound. m/z 456 (M+.).

WORKUP

后处理

  1. additionadded to the reaction mixture
  2. customquenched with acetic acid
  3. customThe solvent was removed in vacuo
  4. customThe residue was purified by silica gel column chromatograhy