HRID1796678
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
A solution of 430F (42 mg, 0.10 mmol), 3-acetylamino-benzoic acid (27 mg, 0.15 mmol), PyBrop (73 mg, 0.15 mmol) and DIEA 70 μl, 0.40 mmol) in DMF (1 ml) was stirred at room temperature for 16 h under argon. Treated with EtOAc (30 ml), the mixture was washed with H2O (3×10 ml) and brine (10 ml), dried with Na2SO4. Removal of the solvent followed by flash chromatography of the residue on silica gel (50% EtOAc-CH2Cl2) gave 430 (38 mg, 70%) as a light yellow solid. It has a retention time of 6.16 min (standard LC1 method, 8 min run). MS Found: (M+H)+=547.2
WORKUP
后处理
- washthe mixture was washed with H2O (3×10 ml) and brine (10 ml)
- dry with materialdried with Na2SO4
- customRemoval of the solvent