HRID2083809
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customthe catalyst was removed
- concentrationconcentrated
- dissolutiondissolved in THF (800 ml.)
- waitAfter 4 hours
- customthe catalyst was removed
- concentrationconcentrated in vacuo
- additionby treating with n-hexane
- customThe solid residue was recrystallized by ethyl acetate - THF - n-hexane