HRID2075967

反应详情

EQUATION

反应方程式

HRID 2075967 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of 5-benzyloxy-4-methoxy-N,N-dimethyl-2-(5-methyl-[1,2,4]oxadiazol-3-yl)benzenesulfonamide and methylene chloride (20 mL) was added titanium(IV) chloride (0.472 g) under ice-bath cooling. After stirring at room temperature overnight, 2 mol/L hydrochloric acid and methylene chloride were added to the mixture. The separated organic layer was washed with 2 mol/L hydrochloric acid and brine successively, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (eluent: 10%-100% ethyl acetate/hexane, gradient elution) to give the title compound (121 mg).

WORKUP

后处理

  1. temperaturecooling
  2. washThe separated organic layer was washed with 2 mol/L hydrochloric acid and brine successively
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was purified by silica gel column chromatography (eluent: 10%-100% ethyl acetate/hexane, gradient elution)