HRID512816

反应详情

EQUATION

反应方程式

HRID 512816 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
27.5 °C

PROCEDURE

实验过程

Added 1-((2S,3S)-2-(benzyloxy)pentan-3-yl)-4-(4-(4-(4-hydroxyphenyl) piperazin-1-yl)phenyl)-1H-1,2,4-triazol-5(4H)-one compound of formula-20 (35 g) to a mixture of dimethylsulfoxide (350 ml) and sodium hydroxide (3.4 g) and water (7 ml) at 25-30° C. and stirred for 45 minutes at 25-30° C. ((3S,5R)-5-((1H-1,2,4-triazol-1-yl)methyl)-5-(2,4-difluorophenyl)tetrahydrofuran-3-yl)methyl-4-methylbenzenesulfonate compound of formula-10 (31.5 g) was added to the above reaction mixture at 25-30° C. and stirred 5 hours at 25-30° C. After completion of the reaction, water was added to the reaction mixture. The reaction mixture was extracted twice with ethyl acetate. The organic layers were washed with 10% sodium chloride solution. Distilled off the solvent under reduced pressure to get the compound as residue. Dissolved the obtained residue in isopropanol (320 ml) at 45-50° C. Filtered the solid, washed with water and dried to get the title compound. Yield: 98%; Purity by HPLC: 95.1%

WORKUP

后处理

  1. additionwas added to the above reaction mixture at 25-30° C.
  2. additionwas added to the reaction mixture
  3. extractionThe reaction mixture was extracted twice with ethyl acetate
  4. washThe organic layers were washed with 10% sodium chloride solution
  5. distillationDistilled off the solvent under reduced pressure
  6. customto get the compound as residue
  7. filtrationFiltered the solid
  8. washwashed with water
  9. customdried