HRID661458

反应详情

EQUATION

反应方程式

HRID 661458 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

The compound obtained in Example 2 (2) above (2.43 g), methoxyamine hydrochloride (1.25 g), sodium acetate (1.64 g) and water (2.4 ml) were added to tetrahydrofuran (22 ml) and the mixture was stirred at room temperature for about 48 hours. Toluene (24 ml) and water (12 ml) were added to the reaction mixture, the organic layer was separated, and washed with water (12 ml) and a saturated brine (12 ml). The organic layer was concentrated at reduced pressure and the resulting residue was purified by column chromatography and concentrated to give the titled compound as an oily material (1.92 g, yield 71%). MS (APCI) m/z: 273 [M+H]+.

WORKUP

后处理

  1. customthe organic layer was separated
  2. washwashed with water (12 ml)
  3. concentrationThe organic layer was concentrated at reduced pressure
  4. customthe resulting residue was purified by column chromatography
  5. concentrationconcentrated