HRID2083809

反应详情

EQUATION

反应方程式

HRID 2083809 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

BOC-Ala-Gly-OBzl (101 g.) was dissolved in THF (500 ml.) and hydrogenized with 5% palladium/carbon (7 g.). After 6 hours, the catalyst was removed, concentrated, dissolved in THF (800 ml.), then again hydrogenized with 5% palladium/carbon. After 4 hours, the catalyst was removed and concentrated in vacuo, and the residue was solidified by treating with n-hexane. The solid residue was recrystallized by ethyl acetate - THF - n-hexane to obtain BOC-Ala-Gly-OH (72 g., Yield: 97.4%, m.p.: 129° - 132° C.). TLC: one spot (solvent system 3). [α]D28 = -8.87° (c=1, DMF).

WORKUP

后处理

  1. customthe catalyst was removed
  2. concentrationconcentrated
  3. dissolutiondissolved in THF (800 ml.)
  4. waitAfter 4 hours
  5. customthe catalyst was removed
  6. concentrationconcentrated in vacuo
  7. additionby treating with n-hexane
  8. customThe solid residue was recrystallized by ethyl acetate - THF - n-hexane