反应详情

4N HCl/dioxane (2 ml) was added to the compound Boc-Asn-Apns-Dmt-NHBzl(2-Me) (70 mg) obtained in the step 1 of Example 6 and the mixture was stirred for two hours. After concentration, the reaction mixture was dissolved in DMF (1 ml) and neutralized with triethylamine (15 μl). After the addition of methyl chloroformate (9 μl ) and triethylamine (16 μl), the mixture was stirred for two hours. After the addition of ethyl acetate, the reaction mixture was washed with 3% Na2CO3, 1N HCl, and 5% NaCl and dried over MgSO4. After filtration and concentration, the residue was purified using silica gel column chromatography to obtain the title compound (15 mg).

1. customobtained in the step 1 of Example 6
2. concentrationAfter concentration
3. dissolutionthe reaction mixture was dissolved in DMF (1 ml)
4. additionAfter the addition of methyl chloroformate (9 μl ) and triethylamine (16 μl)
5. stirringthe mixture was stirred for two hours
6. additionAfter the addition of ethyl acetate
7. washthe reaction mixture was washed with 3% Na2CO3, 1N HCl, and 5% NaCl
8. dry with materialdried over MgSO4
9. filtrationAfter filtration and concentration
10. customthe residue was purified