HRID485316

反应详情

EQUATION

反应方程式

HRID 485316 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of 20.6 ml. (0.24 mole) 37% aqueous formaldehyde, 18 ml. (0.12 mole) 40% aqueous dimethylamine and 80 ml. acetic acid is cooled to 0° and treated by dropwise addition with 25.5 g. (0.113 mole) 2-(5-methyl-3-phenyl-4-isoxazolyl)-indole in a solution of 45 ml. acetic acid and 125 ml. dioxane. After addition is complete the mixture is stirred for 1 hour at room temperature and poured onto 500 ml. ice-water. The resulting solution is made basic with 20% potassium hydroxide and then extracted with methylene chloride. The methylene chloride is washed with water, brine, dried over anhydrous magnesium sulfate, filtered and evaporated to give 2-(5-methyl-3-phenyl-4-isoxazolyl)-3-(dimethylaminomethyl)-indole.

WORKUP

后处理

  1. additionA mixture of 20.6 ml
  2. additiontreated by dropwise addition with 25.5 g
  3. additionAfter addition
  4. additionpoured onto 500 ml
  5. extractionextracted with methylene chloride
  6. washThe methylene chloride is washed with water, brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. customevaporated