HRID2245770

反应详情

EQUATION

反应方程式

HRID 2245770 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 6-benzenesulfonyl-hexa-2,4-dienoic acid (0.292 g, 1.15 mmol) in dry dichloromethane (5 mL) was added dropwise oxalyl chloride, at 0° C. under an atmosphere of argon. One drop on dimethylformamide was then added. After stirring at 2020 C. for one hour, a solution of aqueous hydroxylamine (50%, 0.17 mL, 2.5 mmol) in tetrahydrofuran (5 mL) was added. The mixture was stirred for an additional hour and concentrated under reduced pressure to give a yellow foam that was purified by column chromatography (8:2 ethyl acetate:40-60° C. petroleum to 100% ethyl acetate). The title compound (91 mg, 31%) was obtained as a white foam.

WORKUP

后处理

  1. customat 0° C.
  2. additionOne drop on dimethylformamide was then added
  3. stirringThe mixture was stirred for an additional hour
  4. concentrationconcentrated under reduced pressure
  5. customto give a yellow foam that
  6. customwas purified by column chromatography (8:2 ethyl acetate:40-60° C. petroleum to 100% ethyl acetate)