HRID979238

反应详情

EQUATION

反应方程式

HRID 979238 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

β-Alanine (5 g) in water (50 ml) is added to 3-benzyloxy-2-methyl-4-pyrone (10 g) in 95% ethanol (100 ml) and sodium hydroxide (4 g) in water (50 ml) is then slowly added to the reaction mixture until a pH of 13 is obtained. The solution is refluxed for 15 minutes during which time the colour changes from yellow to amber. After cooling, the solution is acidified to pH 2.5 with concentrated HCl (about 2 ml) and is then rotary evaporated at 50° C. The resulting oil is subjected to a methylene chloride/water extraction. The solid which remains is triturated with acetone and recrystallised from water to give 3-benzyloxy-1-(2'-carboxyethyl)-2-methylpyrid-4-one, m.p. 81°-83° C.

WORKUP

后处理

  1. additionis then slowly added to the reaction mixture until a pH of 13
  2. customis obtained
  3. temperatureThe solution is refluxed for 15 minutes during which time the colour changes from yellow
  4. temperatureAfter cooling
  5. customis then rotary evaporated at 50° C
  6. extractionThe resulting oil is subjected to a methylene chloride/water extraction
  7. customThe solid which remains is triturated with acetone
  8. customrecrystallised from water