HRID1596751

反应详情

EQUATION

反应方程式

HRID 1596751 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dimethylformamide (44 ml), 1-amino-1-(4-methoxycarbonylphenyl)-3-oxo-3-(4-pentyloxyphenyl)-1-propene (5.5 g) and hydroxylamine hydrochloride (2.0 g) were charged in 300-ml three-necked flask at room temperature and heated, and the reaction was carried out at the inner temperature of 55 to 60° C. for 4 hours. After completion of the reaction, the mixture was cooled down to room temperature, and acetonitrile (110 ml) was added to separate the crystals. The inner temperature was made 0 to 5° C., and the crystals were filtered and washed with acetonitrile (28 ml) and water (110 ml) The crystals were dried overnight in vacuo to give methyl 4-[5-(4-pentyloxyphenyl)isoxazol-3-yl]benzoate (5.21 g).

WORKUP

后处理

  1. temperatureheated
  2. customAfter completion of the reaction
  3. customto separate the crystals
  4. customwas made 0 to 5° C.
  5. filtrationthe crystals were filtered
  6. washwashed with acetonitrile (28 ml) and water (110 ml) The crystals
  7. customwere dried overnight in vacuo