反应详情

25 g of H-Ala-OMe, HCl and 66 g. of Boc-Ser-ONb are dissolved in 500 ml DMF. The product is cooled in an ice bath and 25 ml of NEM, 24 g of N-hydroxy benzotriazole are added wtih magnetic stirring and the pH is maintained at 6.5 or 7 by addition of NEM. The product is stirred for 18 hrs. at ambient temperature. After TLC monitoring, the medium is evaporated to 90% (13.33 Pa 35° C.). The oil obtained is dissolved in 1.500 ml of chloroform, the product is washed with a solution of saturated sodium chloride (twice), 5% potassium sulfate/bisulfate solution (3 times), saturated sodium bicarbonate (5 times). The solution is dried over Na2 `SO4 and evaporated to dryness. An oil is obtained which is dried to constant weight (30° C.13.33 Pa)

1. temperatureThe product is cooled in an ice bath
2. temperaturethe pH is maintained at 6.5 or 7 by addition of NEM
3. stirringThe product is stirred for 18 hrs
4. customat ambient temperature
5. customAfter TLC monitoring, the medium is evaporated to 90% (13.33 Pa 35° C.)
6. customThe oil obtained
7. washthe product is washed with a solution of saturated sodium chloride (twice), 5% potassium sulfate/bisulfate solution (3 times), saturated sodium bicarbonate (5 times)
8. customThe solution is dried over Na2 `SO4
9. customevaporated to dryness
10. customAn oil is obtained which
11. customis dried to constant weight (30° C.13.33 Pa)