反应详情

The compound (185.8 mg) obtained in Example 65-1 was dissolved in a small amount of water. The solution was added with chloroform and a 1 mol/l sodium hydroxide aqueous solution, and the organic layer and an oily substance were collected, followed by drying with anhydrous magnesium sulfate. After filtration, the solvent was distilled off. An anhydrous DMF solution (2 ml) containing the resultant sodium salt (143.6 mg) and N-(2-hydroxyethyl)morpholine (38 mg) was added with HOBt (37 mg) and WSCI hydrochloride (63 mg) and the whole was stirred overnight. After the solvent was distilled off, the resultant was dissolved in chloroform and washed with a saturated aqueous sodium hydrogen carbonate solution. The aqueous layer was extracted with chloroform and dried with anhydrous magnesium sulfate. The reaction mixture obtained by distillating the solvent off was purified through silica gel column chromatography (chloroform). The resultant was dissolved in dioxane and a salt was allowed to precipitate with a 4 mol/l hydrogen chloride/dioxane solution. After the solvent was distilled off, the solid substance was pulverized and dried under reduced pressure, thereby obtaining a hydrochloride (143,4 mg) of the subject compound as a white solid.

1. customa 1 mol/l sodium hydroxide aqueous solution, and the organic layer and an oily substance were collected
2. dry with materialby drying with anhydrous magnesium sulfate
3. filtrationAfter filtration
4. distillationthe solvent was distilled off
5. additionAn anhydrous DMF solution (2 ml) containing the resultant sodium salt (143.6 mg) and N-(2-hydroxyethyl)morpholine (38 mg)
6. additionwas added with HOBt (37 mg) and WSCI hydrochloride (63 mg)
7. distillationAfter the solvent was distilled off
8. dissolutionthe resultant was dissolved in chloroform
9. washwashed with a saturated aqueous sodium hydrogen carbonate solution
10. extractionThe aqueous layer was extracted with chloroform
11. dry with materialdried with anhydrous magnesium sulfate
12. customThe reaction mixture obtained
13. customoff was purified through silica gel column chromatography (chloroform)
14. dissolutionThe resultant was dissolved in dioxane
15. customto precipitate with a 4 mol/l hydrogen chloride/dioxane solution
16. distillationAfter the solvent was distilled off
17. customdried under reduced pressure