反应详情

To 4.4 g. of the 4-(2-acetamidomethylpropan-2-yl)-1,2-diaminobenzene (prepared in Example 1f) in 120 ml. dry dichloromethane are added 3.3 ml. triethylamine and then, with ice cooling, 3.06 g. 4-methylbenzoic acid chloride. After stirring the reaction mixture for 3 hours at ambient temperature, the solvent is removed in a vacuum. The residue is dissolved in water and extracted three times with dichloromethane, the organic phase is dried over anhydrous sodium sulphate, filtered and the solvent is removed in a vacuum. The residue (6.7 g.) is dissolved in glacial acetic acid and stirred for 3 hours at 70° C. The solvent is removed in a vacuum and the residue is purified by column chromatography (silica gel; dichloromethane containing 5% methanol). There is obtained 1.55 g. of the title compound; m.p. 230°-232° C.

1. customthe solvent is removed in a vacuum
2. dissolutionThe residue is dissolved in water
3. extractionextracted three times with dichloromethane
4. dry with materialthe organic phase is dried over anhydrous sodium sulphate
5. filtrationfiltered
6. customthe solvent is removed in a vacuum
7. dissolutionThe residue (6.7 g.) is dissolved in glacial acetic acid
8. stirringstirred for 3 hours at 70° C
9. customThe solvent is removed in a vacuum
10. customthe residue is purified by column chromatography (silica gel; dichloromethane containing 5% methanol)
11. customThere is obtained 1.55 g