Lithium Hydroxide → 4-{(3R)-3-[(4-{[(3,4-Dichlorophenyl)amino]carbonyl}piperazin-1-yl)methyl]piperidin-1-yl}butanoic acid

To a solution of methyl 4-{(3R)-3-[(4-{[(3,4-dichlorophenyl)amino]carbonyl}piperazin-1-yl)methyl]piperidin-1-yl}butanoate (80 mg) in tetrahydrofuran (5 mL) was added 1M aqueous lithium hydroxide (1 mL). The mixture was stirred overnight at room temperature. The mixture was then loaded directly onto an SCX-2 column and eluted with methanol then 7M NH3 in methanol. The basic fraction was concentrated at reduced pressure and the residue was purified using reverse phase HPLC eluting with a mixture of 5-95% acetonitrile in water and then SCX-2 column eluting with methanol then 7M NH3 in methanol to give the title compound as a white solid (60 mg, 77%).

1. washeluted with methanol
2. concentrationThe basic fraction was concentrated at reduced pressure
3. customthe residue was purified
4. washeluting with a mixture of 5-95% acetonitrile in water
5. washSCX-2 column eluting with methanol

ORD 기록

ord-41a15351811d4f1a9f08994ffa6488e8

출처 데이터셋

uspto-grants-2014_04

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08710224B2