反应详情

温度

-15 °C

5.06 Grams of Z-Ser-NHNH2 was dissolved in 50 ml of dimethylformamide with 6.66 ml of 6N-hydrochloric acid/dioxane, the solution was cooled to -15° C. then 2.68 ml of isoamyl nitrite was added thereto, and the mixture was stirred for 5 minutes. Next, 5.60 ml of triethylamine was added to neutralize the reaction mixture. This reaction mixture was added to 30 ml of dimethylformamide solution containing 3.11 g of H-Ser-OMe.HCl and 2.80 ml of triethylamine, then this mixture was stirred at 4° C. for 20 hours. Dimethylformamide was removed by distillation, the residue obtained was extracted with ethyl acetate, the extract was washed with water and was dried with anhydrous sodium sulfate. After removal of ethyl acetate by distillation, the residue was crystallized by adding ether, reprecipitated from ethyl acetate-ether to obtain 3.75 g of Z-Ser-Ser-OMe.

1. stirringthis mixture was stirred at 4° C. for 20 hours
2. customDimethylformamide was removed by distillation
3. customthe residue obtained
4. extractionwas extracted with ethyl acetate
5. washthe extract was washed with water
6. dry with materialwas dried with anhydrous sodium sulfate
7. customAfter removal of ethyl acetate
8. distillationby distillation
9. customthe residue was crystallized
10. additionby adding ether
11. customreprecipitated from ethyl acetate-ether