HRID456890

反应详情

EQUATION

反应方程式

HRID 456890 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A mixture of 2-chloro-N-(1-hydroxy-cycloheptylmethyl)-5-(hydroxyimino-methyl)-benzamide (50 mg, 0.15 mmol), but-3-yn-1-ol (27 mg, 0.38 mmol), sodium hypochlorite (1 mL, 4%) and triethylamine (2 drops) in dichloromethane (2 mL) was stirred at room temperature for 5 d. The mixture was diluted with water and extracted with ethyl acetate. The combined organic layers were washed with water, and brine, dried over sodium sulfate, filtered and adsorbed onto silica gel. The residue was purified by flash column chromatography (65% ethyl acetate-hexanes) to afford the title compound (13 mg).

WORKUP

后处理

  1. extractionextracted with ethyl acetate
  2. washThe combined organic layers were washed with water, and brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. customThe residue was purified by flash column chromatography (65% ethyl acetate-hexanes)