反应详情

The free base form of N1-[2-(2-aminoethoxy)-4-methoxybenzoyl]-N2-(4-methoxybenzoyl)-1,2-benzenediamine was prepared by vigorously stirring N1-[2-(2-aminoethoxy)-4-methoxybenzoyl]-N2-(4-methoxybenzoyl)-1,2-benzenediamine trifluoroacetate (1.88 g, 3.42 mmol) with 100 ml water, 2 grams potassium carbonate and 100 ml of CH2Cl2 for several hours at room temperature. After stirring, the organic layer was set aside and combined with a 150 ml CH2Cl2 wash of the original aqueous layer. The combined CH2Cl2 extracts were washed with brine, dried over Na2SO4, concentrated in vacuo, then purified on a chromatotron system (4 mm plate) with 9:1 CH2Cl2:MeOH eluent to provide N1-[2-(2-aminoethoxy)-4-methoxybenzoyl]-N2-(4-methoxybenzoyl)-1,2-benzenediamine (1.26 g, 85%) as a brittle white foam after high vacuum drying.

1. washwash of the original aqueous layer
2. washThe combined CH2Cl2 extracts were washed with brine
3. dry with materialdried over Na2SO4
4. concentrationconcentrated in vacuo
5. custompurified on a chromatotron system (4 mm plate) with 9:1 CH2Cl2