反应详情

2 g of the Boc-Gln Resin obtained in Step 4 is put in 160 ml of acetic acid and allowed to stand for 6 hours at room temperature. The mixture is filtered with a glass filter. The cake is put in 160 ml of acetic acid, agitated and filtered. This operation is repeated three times. Then, the cake is agitated in 160 ml of 1N aqueous HCl/acetic acid at room temperature for half an hour to remove the Boc group from the resin. The resulting product is filtered off, washed with three portions of each of acetic acid, ethanol and dimethylformamide successively, and agitated in 160 ml of a 10% by weight solution of triethylamine in dimethylformamide to effect neutralization reaction. The resulting product is filtered off and washed with each of dimethylformamide and methylene chloride. The product is immersed in a solution made by adding 2 mmol of Boc-serine (Bzl) to 12 ml of methylene chloride, and agitated. Ten minutes later, a solution made by adding 20 mmol of dicyclohexyl carbodiimide to 60 ml of methylene chloride is added to the mixture and agitated at room temperature for 2 hours to effect coupling reaction. The resulting product is filtered off and washed with each of methylene chloride and ethanol.

1. filtrationThe mixture is filtered with a glass
2. filtrationfilter
3. filtrationfiltered
4. stirringThen, the cake is agitated in 160 ml of 1N aqueous HCl/acetic acid at room temperature for half an hour
5. customto remove the Boc group from the resin
6. filtrationThe resulting product is filtered off
7. washwashed with three portions of each of acetic acid, ethanol and dimethylformamide successively
8. stirringagitated in 160 ml of a 10% by weight solution of triethylamine in dimethylformamide
9. customreaction
10. filtrationThe resulting product is filtered off
11. washwashed with each of dimethylformamide and methylene chloride
12. stirringagitated
13. customTen minutes
14. additionis added to the mixture
15. stirringagitated at room temperature for 2 hours
16. customreaction
17. filtrationThe resulting product is filtered off
18. washwashed with each of methylene chloride and ethanol