HRID2369797

反应详情

EQUATION

反应方程式

HRID 2369797 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

17-{3-[tert-Butoxycarbonyl (2-carboxyethyl)amino]propionylamino}heptadecanoic acid tert-butyl ester (0.122 g, 0.2 mmol) was dissolved in THF (5 mL). DIEA (39 ul) was added and the mixture was cooled to 0° C. TSTU (66 mg, 0.22 mmol) was added. The mixture was stirred at 0° C. for 30 min, then for 16 h at RT. The mixture was concentrated under vacuum. AcOEt (15 mL) and the solution was washed with 0.2 N HCl (5 ml) and sat. NaCl (5 ml), dried over MgSO4, and dried under vacuum. The residue was purified by flash chromatography (silica) eluting with AcOEt/heptane (9:1) and AcOEt. The appropriate fractiones were pooled and concentrated under vacuum to yield 58 mg.

WORKUP

后处理

  1. waitfor 16 h at RT
  2. concentrationThe mixture was concentrated under vacuum
  3. washAcOEt (15 mL) and the solution was washed with 0.2 N HCl (5 ml) and sat. NaCl (5 ml)
  4. dry with materialdried over MgSO4
  5. customdried under vacuum
  6. customThe residue was purified by flash chromatography (silica)
  7. washeluting with AcOEt/heptane (9:1) and AcOEt
  8. concentrationconcentrated under vacuum
  9. customto yield 58 mg