反应详情

In 20 ml of ethyl alcohol is dissolved 4.7 g of BOC-(D)-Met-Gly-OEt. After cooling, 16 ml of N-aqueous sodium hydroxide solution is added, and the mixture is stirred at room temperature for 1 hour. The ethyl alcohol is distilled off, and the residue, after adding aqueous citric acid solution to neutralize, is extracted with 100 ml of ethyl acetate, followed by washing with water and drying over anhydrous sodium sulphate. The AcOEt isdistilled off and the residue is crystallized with petroleum ether. Recrystallization from AcOEt-petroleum ether results in a yield of 3.8 g of the desired product, m.p. 124°-125° C., Rf1 =0.41, [α]D21 +12.3° (c=0.59, DMF)

1. temperatureAfter cooling
2. distillationThe ethyl alcohol is distilled off
3. additionthe residue, after adding aqueous citric acid solution
4. extractionis extracted with 100 ml of ethyl acetate
5. washby washing with water
6. dry with materialdrying over anhydrous sodium sulphate
7. customthe residue is crystallized with petroleum ether
8. customRecrystallization from AcOEt-petroleum ether