HRID882690

反应详情

EQUATION

反应方程式

HRID 882690 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of Boc-Val-Pro-OH (94.5 mg, 0.30 mmol) in dimethylformamide (1.5 mL), was successively treated, at room temperature, with 1-hydroxibenzotriazol (40.5 mg, 0.30 mmol), N,N-diisopropylcarbodiimide (46.7 μL, 0.30 mmol) and Ara-C (60.9 mg, 0.25 mmol). The stirring was continued until complete disappearance of the starting material (overnight stirring). Then, the solvent was evaporated, the residue was dissolved in ethyl acetate and washed with citric acid (10%), NaHCO3 (10%) and brine. The organic layer was dried (Na2SO4) and evaporated to give a residue that was purified by CCTLC on the chromatotron with dichloromethane:methanol (20:1) to yield Ara-C-dipeptide (A) (21% yield)

WORKUP

后处理

  1. customThen, the solvent was evaporated
  2. dissolutionthe residue was dissolved in ethyl acetate
  3. washwashed with citric acid (10%), NaHCO3 (10%) and brine
  4. dry with materialThe organic layer was dried (Na2SO4)
  5. customevaporated
  6. customto give a residue that
  7. customwas purified by CCTLC on the chromatotron with dichloromethane:methanol (20:1)