1-Hydroxybenzotriazole → HCID 68818466, 화합물

1-(tert-Butoxycarbonyl)-piperidine4-carboxylic acid (0.53 g), (S)-1-benzyloxycarbonyl-3-methylpiperazine (D19)(0.5 g), HOBt (0.29 g) and diethylaminomethyl polystyrene (1.78 g) were stirred in DCM (30 ml), then EDC (0.53 g) was added and the reaction was stirred at rt ovemight. The mixture was filtered and washed with saturated sodium hydrogen carbonate solution (3×50 ml) and brine (30 ml). The organic layer was dried (MgSO4) and evaporated to give a crude yellow oil which was purified by chromatography [silica gel; 0-100% ethyl acetate/hexane) to give the tide compound (D20) as a clear oil which crystallised on standing (0.88 g).

1. filtrationThe mixture was filtered
2. washwashed with saturated sodium hydrogen carbonate solution (3×50 ml) and brine (30 ml)
3. dry with materialThe organic layer was dried (MgSO4)
4. customevaporated
5. customto give a crude yellow oil which
6. customwas purified by chromatography [silica gel
7. custom0-100% ethyl acetate/hexane) to give the tide compound (D20) as a clear oil which
8. customcrystallised

ORD 기록

ord-a9d13b3a961346c3b33f3099d5c8fce9

출처 데이터셋

uspto-grants-2009_09

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07592347B2