HRID467354

反应详情

EQUATION

反应方程式

HRID 467354 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To 7.4 g H-Gly-OBzl.p-Tos-OH, 100 ml acetonitrile was added, and this was followed by cooling with ice, then 3.1 ml TEA, 3.78 g Boc-D-Ala-OH, 3.96 g HONB and 4.54 g DCC were added, and this was followed by agitation for one night. The resulting DCU was filtered, and the filtrate was concentrated, then the resulting residue was dissolved in 300 ml AcOEt. The resulting solution was washed with 4% aqueous NaHCO3 and 10% aqueous citrate, after which it was dried with Na2SO4. The dried product, after concentration, was crystallized with petroleum benzine and collected by filtration.

WORKUP

后处理

  1. temperatureby cooling with ice
  2. waitthis was followed by agitation for one night
  3. filtrationThe resulting DCU was filtered
  4. concentrationthe filtrate was concentrated
  5. dissolutionthe resulting residue was dissolved in 300 ml AcOEt
  6. washThe resulting solution was washed with 4% aqueous NaHCO3 and 10% aqueous citrate
  7. dry with materialafter which it was dried with Na2SO4
  8. concentrationThe dried product, after concentration
  9. customwas crystallized with petroleum benzine
  10. filtrationcollected by filtration