HRID1425656

反应详情

EQUATION

反应方程式

HRID 1425656 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-[9-(2,5-Dioxopyrrolidin-1-yloxycarbonyl)nonyloxy]benzoic acid tert-butyl ester (200 mg, 0.433 mmol) was stirred in DMF (2 mL) and H-Glu-NH2 (63 mg) was added. The non-homogeneous mixture was stirred at rt for 16 h. LC/MS analysis indicated the reaction had not gone to completion. H-Glu-NH2 (20 mg) and more DMF (2 mL) were added and the mixture was stirred for 2 d at rt. The sample was concentrated under vacuum and AcOEt (50 mL) was added. The solution was washed with 0.2 N HCl (2×25 mL) and water (25 mL), dried over MgSO4, and concentrated under vacuum to yield a white solid (180 mg, 86% yield).

WORKUP

后处理

  1. stirringthe mixture was stirred for 2 d at rt
  2. concentrationThe sample was concentrated under vacuum and AcOEt (50 mL)
  3. additionwas added
  4. washThe solution was washed with 0.2 N HCl (2×25 mL) and water (25 mL)
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under vacuum