HRID2265106

反应详情

EQUATION

反应方程式

HRID 2265106 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
120 °C

PROCEDURE

实验过程

Compound 14b (14.6 mg) was dissolved in toluene (132 ml), and (carbetoxyethylidene)triphenylphosphorane (46.9 g) was added thereto. The obtained mixture was stirred under heating at 120° C. for 2 hours. After the reaction mixture was allowed to cool, n-heptane was added thereto and stirred. The precipitated solid was filtered off, and the filtrate was concentrated under reduced pressure. The obtained residue was dissolved in methanol (125 ml), and purified water was added thereto. The precipitated solid was filtered off and then dried under reduced pressure. Thus, Compound 14c (17.3 g, 79%) was obtained as an opalescent solid.

WORKUP

后处理

  1. temperatureto cool
  2. stirringstirred
  3. filtrationThe precipitated solid was filtered off
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. dissolutionThe obtained residue was dissolved in methanol (125 ml)
  6. custompurified water
  7. additionwas added
  8. filtrationThe precipitated solid was filtered off
  9. customdried under reduced pressure