反应详情

A solution of (R)-(1,1-dimethylethyl 2-{[(3-{2-[4-(2-methyl-5-quinolinyl)-1-piperazinyl]ethyl}phenyl)amino]methyl}-1-pyrrolidinecarboxylate in methanol was treated with absolution of hydrogen chloride in ether (1 M). The resulting mixture was stirred 30 minutes then concentrated under vacuum and then loaded onto an ion-exchange cartridge (SCX-2) and eluted with methanol followed by ammonia in methanol (1 M). The combined basic fractions were concentrated under vacuum. The residue, (10 mg) was then dissolved in DCM (1 mL) and treated with triphosgene (23 mg, 0.3 eq.), diisopropylamine (4 uL, 3 eq.). The mixture was stirred for 1 h then concentrated under vacuum and purified by preparative mass-directed hplc to afford the title compound (3.1 mg).

1. concentrationthen concentrated under vacuum
2. washeluted with methanol
3. concentrationThe combined basic fractions were concentrated under vacuum
4. dissolutionThe residue, (10 mg) was then dissolved in DCM (1 mL)
5. stirringThe mixture was stirred for 1 h
6. concentrationthen concentrated under vacuum
7. custompurified by preparative mass-directed hplc