反应详情

Next, 31.3 g (0.08 mole) of H-Arg(NO2)-CHA.HCl was dissolved in 160 ml of 1.5N-NEM/DMF, to this solution was added 31.0 g (0.08 mole) of BOC-Phe-SDP (dimethylmercaptopyrimidine) at 0° to 5° C. and reacted for 18 hours. After the reaction was completed, the reaction mixture was diluted with 1600 ml of AcOEt, and washed twice with 400 ml of cold 5% hydrochloric acid, and washed twice with 400 ml of an aqueous solution saturated with sodium chloride, then there was precipitated crystals. The crystals thus precipitated were collected by filtration and dried to obtain crude BOC-Phe-Arg(NO2)-CHA, then recrystallized from AcOEt/n-hexane to obtain 35.1 g (72.9%) of BOC-Phe-Arg(NO2)-CHA.

1. customreacted for 18 hours
2. washwashed twice with 400 ml of cold 5% hydrochloric acid
3. washwashed twice with 400 ml of an aqueous solution saturated with sodium chloride
4. customthere was precipitated crystals
5. customThe crystals thus precipitated
6. filtrationwere collected by filtration
7. customdried