HRID1425656
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- stirringthe mixture was stirred for 2 d at rt
- concentrationThe sample was concentrated under vacuum and AcOEt (50 mL)
- additionwas added
- washThe solution was washed with 0.2 N HCl (2×25 mL) and water (25 mL)
- dry with materialdried over MgSO4
- concentrationconcentrated under vacuum