Dicyclohexylcarbodiimide → D-Lysine

One half (0.5) mmol of BOC3(DTPA) was dissolved in 10 ml DCM. 0.6 mmol of DCC was dissolved in 5 ml DCM and added to the BOC3(DTPA) mixture. The reaction was carried out for 1 hour at room temperature. The white crystals that appeared in the mixture were filtered out. 0.5 mmol of solid BOC-Lys-OtBu was added to the reaction. The reaction was carried out for 20 hours at room temperature. The mixture was filtered and the DCM was evaporated. The product was washed several times with ethanol and air-dried. Cleavage of the protecting groups (BOC, OtBu) was carried out in 1 ml TFA (trifluoroacetic acid)+5% water for 3 hours. The acid was evaporated in a vacuum over a KOH pellet. The final product D-Lys(DTPA) was washed several times with diethyl ether and dried. D-Lys(DTPA) was dissolved in water and lyophilized.

1. filtrationwere filtered out
2. waitThe reaction was carried out for 20 hours at room temperature
3. filtrationThe mixture was filtered
4. customthe DCM was evaporated
5. washThe product was washed several times with ethanol
6. customair-dried
7. waitCleavage of the protecting groups (BOC, OtBu) was carried out in 1 ml TFA (trifluoroacetic acid)+5% water for 3 hours
8. customThe acid was evaporated in a vacuum over a KOH pellet
9. washThe final product D-Lys(DTPA) was washed several times with diethyl ether
10. customdried
11. dissolutionD-Lys(DTPA) was dissolved in water

ORDレコード

ord-b976a72da8f34afebb95baffbcbbfb1f

出典データセット

uspto-grants-2015_03

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08993278B2