反应详情

Triethylamine (0.25 mL), dimethylamine hydrochloride (133 mg), 1-hydroxybenzotriazole monohydrate (53 mg) and 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (75 mg) were added to a chloroform suspension (10 mL) of the compound (168 mg) obtained in Example 56, and the mixture was stirred for 72 hours. The solvent was distilled away under reduced pressure. Water was added to the residue, and the mixture was extracted with chloroform. The resultant organic layer was washed with saturated brine and dried over magnesium sulfate anhydrate. The solvent was distilled away under reduced pressure, and the resultant residue was purified by silica gel column chromatography (methylene chloride:methanol=93:7). The thus-obtained colorless solids (135 mg) were suspended in ethanol (5 mL), and then 1N HCl in ethanol (0.5 mL) was added. The mixture was stirred for 2 hours, and the solvent was distilled away to give the title compound (112 mg).

1. distillationThe solvent was distilled away under reduced pressure
2. additionWater was added to the residue
3. extractionthe mixture was extracted with chloroform
4. washThe resultant organic layer was washed with saturated brine
5. dry with materialdried over magnesium sulfate anhydrate
6. distillationThe solvent was distilled away under reduced pressure
7. customthe resultant residue was purified by silica gel column chromatography (methylene chloride:methanol=93:7)
8. addition1N HCl in ethanol (0.5 mL) was added
9. stirringThe mixture was stirred for 2 hours
10. distillationthe solvent was distilled away