HRID13849
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
To the product of EXAMPLE 91 (30 mg) in THF (1 mL) was added 3 mL of NH3 in methanol (7 M). The reaction stirred for about 15 hours at room temperature before it was concentrated. The residue was dissolved in CH2Cl2 and washed with water. The solution was dried (Na2SO4) and concentrated. The concentrated residue was purified by preparative TLC on silica gel eluted with 100% EtOAc affording the title compound. HPLC/MS: 473.0 (M+1), 475.0 (M+3); Rt=4.19 min.
WORKUP
后处理
- concentrationwas concentrated
- dissolutionThe residue was dissolved in CH2Cl2
- washwashed with water
- dry with materialThe solution was dried (Na2SO4)
- concentrationconcentrated
- customThe concentrated residue was purified by preparative TLC on silica gel
- washeluted with 100% EtOAc affording the title compound