HRID507433

反应详情

EQUATION

反应方程式

HRID 507433 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Burgess reagent (0.8 g, 3.3 mmol) was added in portions to a solution of 5 (0.5 g, 1.58 mmol) in dry THF (20 mL) at room temperature, and was stirred overnight. The mixture was washed with water (20 mL), dried over Na2SO4, concentrated and purified by column chromatography on silica gel to produce compound 6 (0.2 g, 50%) 1H NMR (400 MHz, CDCl3) δ1.44 (s, 9 H), 2.08-2.11 (m, 1 H), 3.17-3.21 (m, 1H), 3.68 (d, 2 H), 4.50-4.60 (m, 1 H), 5.07 (s, 1 H), 5.14 (t, 1 H), 5.37 (t, 1 H).

WORKUP

后处理

  1. washThe mixture was washed with water (20 mL)
  2. dry with materialdried over Na2SO4
  3. concentrationconcentrated
  4. custompurified by column chromatography on silica gel