反应详情

The compound (273.0 mg) obtained in Example 84-2 was dissolved in ethanol (2.7 ml) and added with a 4 mol/l hydrogen chloride/dioxane solution (2.7 ml) and the whole was stirred at room temperature for 1 hour. Further, the solution was added with a 4 mol/l hydrogen chloride/dioxane solution (1.0 ml) and the whole was stirred at room temperature for 30 minutes. After completion of the reaction, the solvent was distilled off, thereby obtaining a crude product (350.0 mg) of [(4-amino-butyl)-propyl-amino]-acetic acid ethyl ester as a colorless oily substance. The resultant crude product (350.0 mg) was dissolved in ethanol (4.5 ml) and added with an ethanol solution (2.6 ml) containing the compound (258 mg) obtained in Example 84-5, acetic acid (0.10 ml), and sodium triacetoxyborohydride (267.0 mg) and the whole was stirred at room temperature for 2 hours. After completion of the reaction, the solvent was distilled off. The residue was dissolved in chloroform and washed with a 1 mol/l sodium hydroxide aqueous solution, followed by extraction with chloroform. The organic layer was washed with a saturated saline solution and dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off. The residue was purified through silica gel column chromatography (chloroform/methanol), thereby obtaining the subject compound (238.0 mg) as a pale-yellow oily substance.

1. stirringthe whole was stirred at room temperature for 30 minutes
2. customAfter completion of the reaction
3. distillationthe solvent was distilled off
4. customobtaining a crude product (350.0 mg) of [(4-amino-butyl)-propyl-amino]-acetic acid ethyl ester as a colorless oily substance
5. stirringthe whole was stirred at room temperature for 2 hours
6. customAfter completion of the reaction
7. distillationthe solvent was distilled off
8. dissolutionThe residue was dissolved in chloroform
9. washwashed with a 1 mol/l sodium hydroxide aqueous solution
10. extractionfollowed by extraction with chloroform
11. washThe organic layer was washed with a saturated saline solution
12. dry with materialdried with anhydrous sodium sulfate
13. filtrationAfter filtration
14. distillationthe solvent was distilled off
15. customThe residue was purified through silica gel column chromatography (chloroform/methanol)