HRID133100

反应详情

EQUATION

反应方程式

HRID 133100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

41.95 g of methyl 3-(4-methoxypyridin-2-yl)propionate (compound F2) are dissolved in 700 ml of tetrahydrofuran, and 217 ml of 1N sodium hydroxide solution are added. The mixture is stirred at RT until no more starting material is detectable (TLC). The mixture is neutralized using 217 ml of 1N hydrochloric acid solution, evaporated to dryness using a rotary evaporator and dried under high vacuum. The colorless residue is ground and extracted four times with dichloromethane/methanol (9:1). The combined extracts are evaporated to dryness. This gives 332 g of the title compound as a colorless powder of m.p. 131-132° C. The mass spectrum shows the molecular peak MH+ at 182 Da

WORKUP

后处理

  1. customevaporated to dryness
  2. customa rotary evaporator
  3. customdried under high vacuum
  4. extractionextracted four times with dichloromethane/methanol (9:1)
  5. customThe combined extracts are evaporated to dryness