HRID1642627
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 N-(t-butoxycarbonylsulfamoyl)-N-(2-benzyloxy-4-phenoxyphenyl)glycine methyl ester (0.375 g, 0.69 mmol) in 6 mL TFA/DCM (1:1) is stirred at ambient temperature for 20 min. The solvent is removed under reduced pressure. Methylene chloride is added to the residue and removed under reduced pressure. The resulting oil is purified by flash chromatography using 10% EtOAc/DCM to elute N-sulfamoyl-N-(2-benzyloxy-4-phenoxyphenyl)glycine methyl ester as an oil: 1H NMR (CDCl3) δ 7.44 (d, J=8.59 Hz, 1H), 7.33-7.26 (m, 7H), 7.09 (t, 1H), 6.97-6.93 (m, 2H), 6.60 (d, J=2.52 Hz, 1H), 6.43 (dd, J=8.59, 2.53 Hz, 1H), 4.96 (s, 2H), 4.26 (s, 2H), 3.62 (s, 3H); MS (M−H)−=441.
WORKUP
后处理
- customThe solvent is removed under reduced pressure
- additionMethylene chloride is added to the residue
- customremoved under reduced pressure
- customThe resulting oil is purified by flash chromatography
- washto elute N-sulfamoyl-N-(2-benzyloxy-4-phenoxyphenyl)glycine methyl ester as an oil