HRID33225

反应详情

EQUATION

反应方程式

HRID 33225 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

4-[1,3]Dioxan-2-yl-N-methyl-butyramide (1 g, 5.35 mmol) was cooled to −78° C. in dry dichloromethane (10 ml) under argon and phosphorus oxychloride (0.65 ml, 7 mmol) was added dropwise. The mixture was warmed to room temperature to give an amber solution which was re-cooled to 0° C. This solution was added dropwise to a suspension of 2-methyl-quinoline-6-carboxylic acid hydrazide (1 g, 5 mmol) in chloroform (20 ml) and the mixture stirred at room temperature overnight. The mixture was poured into water (300 ml), basified with sodium hydroxide solution (5M) and extracted with dichloromethane (3×200 ml). The combined organic portions were dried (Na2SO4), filtered and evaporated to give the desired compound as a brown oil (1.28 g, 83%).

WORKUP

后处理

  1. customto give an amber solution which
  2. temperaturewas re-cooled to 0° C
  3. extractionextracted with dichloromethane (3×200 ml)
  4. dry with materialThe combined organic portions were dried (Na2SO4)
  5. filtrationfiltered
  6. customevaporated