反应详情

The compound (300 mg) obtained in Example 18-2, WSCI hydrochloride (365 mg), and HOBt (260 mg) were dissolved in chloroform (6.0 ml), and the whole was stirred for 1 hour. Then, 3,4-diaminobenzoic acid methyl ester (198 mg) was added thereto and the whole was stirred for 2 hours. A solid was precipitated, so DMF (2.0 ml) was added thereto and stirring was continued for additional 4 hours. After completion of the reaction, the solvent was distilled off under reduced pressure. Then, the residue was dissolved in chloroform and washed with a saturated ammonium chloride aqueous solution, a saturated aqueous sodium hydrogen carbonate solution, and a saturated saline solution. Then, the resultant was dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure. The residue was purified through silica gel column chromatography (chloroform/methanol), thereby obtaining the subject compound (381 mg) as a brown oily substance.

1. stirringthe whole was stirred for 2 hours
2. customA solid was precipitated
3. additionso DMF (2.0 ml) was added
4. stirringstirring
5. waitwas continued for additional 4 hours
6. customAfter completion of the reaction
7. distillationthe solvent was distilled off under reduced pressure
8. dissolutionThen, the residue was dissolved in chloroform
9. washwashed with a saturated ammonium chloride aqueous solution
10. dry with materialThen, the resultant was dried with anhydrous sodium sulfate
11. filtrationAfter filtration
12. distillationthe solvent was distilled off under reduced pressure
13. customThe residue was purified through silica gel column chromatography (chloroform/methanol)